Home Crystal structure of bis(μ2-benzoato-k2O:O′)-bis(μ2-benzoato-k3O,O′:O′)dinitrato-k2O,O′-bis(phenanthroline-k2 N,N′)dierbium(III), C52H36Er2N6O14
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Crystal structure of bis(μ2-benzoato-k2O:O′)-bis(μ2-benzoato-k3O,O′:O′)dinitrato-k2O,O′-bis(phenanthroline-k2 N,N′)dierbium(III), C52H36Er2N6O14

  • Zhang Li ORCID logo EMAIL logo , Yu Hai-yan , Wang Ying-lei , Li Ru-lin and Cao Ying-han
Published/Copyright: July 6, 2022
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Zeitschrift für Kristallographie - New Crystal Structures
From the journal Zeitschrift für Kristallographie - New Crystal Structures Volume 237 Issue 5

Abstract

C52H36Er2N6O14, triclinic, P 1 ‾ (no. 2), a = 10.6499(5) Å, b = 11.0111(5) Å, c = 11.0380(6) Å, α = 85.030(4)°, β = 81.502(4)°, γ = 68.925(4)°, V = 1193.77(11) Å3, Z = 2, R gt (F) = 0.0263, wR ref (F 2) = 0.0592, T = 150.0 K.

CCDC no.: 2180392

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: Pink block
Size: 0.23 × 0.15 × 0.12 mm
Wavelength: Mo Kα radiation (0.71073 Å)
μ: 3.57 mm−1
Diffractometer, scan mode: Xcalibur, ω
θ max, completeness: 26.4°, >99%
N(hkl)measured, N(hkl)unique, R int: 8402, 4875, 0.023
Criterion for I obs, N(hkl)gt: I obs > 2 σ(I obs), 4318
N(param)refined: 334
Programs: CrysAlisPRO [1], Olex2 [2], SHELX [3, 4]
Table 2:

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

Atom x y z U iso*/U eq
Er1 0.62749 (2) 0.49462 (2) 0.35076 (2) 0.02363 (6)
O1 0.7367 (2) 0.3681 (2) 0.5096 (2) 0.0306 (6)
O2 0.4977 (3) 0.3730 (2) 0.4412 (2) 0.0308 (6)
O3 0.5891 (2) 0.3603 (2) 0.6743 (2) 0.0285 (6)
O4 0.3486 (3) 0.3222 (2) 0.5738 (2) 0.0328 (6)
O5 0.7569 (3) 0.3118 (3) 0.2250 (3) 0.0362 (6)
O6 0.5561 (3) 0.4124 (3) 0.1753 (3) 0.0373 (6)
N1 0.8757 (3) 0.4901 (3) 0.3003 (3) 0.0278 (7)
N2 0.6678 (4) 0.3224 (3) 0.1541 (3) 0.0344 (8)
N3 0.6804 (3) 0.6131 (3) 0.1519 (3) 0.0265 (7)
C1 0.4309 (3) 0.2986 (3) 0.4786 (3) 0.0246 (8)
O7 0.6936 (3) 0.2469 (3) 0.0713 (3) 0.0552 (9)
C2 0.7051 (4) 0.3212 (3) 0.6129 (3) 0.0252 (8)
C3 0.9061 (4) 0.5616 (3) 0.2027 (3) 0.0277 (8)
C4 0.8035 (4) 0.6271 (3) 0.1241 (3) 0.0273 (8)
C5 0.5896 (4) 0.6686 (4) 0.0755 (4) 0.0354 (9)
H5 0.506615 0.656583 0.092396 0.042*
C6 0.4526 (4) 0.1803 (3) 0.4090 (3) 0.0287 (8)
C7 0.8142 (4) 0.2112 (3) 0.6677 (3) 0.0266 (8)
C8 0.9712 (4) 0.4306 (4) 0.3704 (4) 0.0382 (10)
H8 0.950884 0.381181 0.437978 0.046*
C9 0.8331 (4) 0.7003 (4) 0.0208 (4) 0.0398 (10)
C10 0.7931 (4) 0.1676 (4) 0.7871 (4) 0.0353 (9)
H10 0.709946 0.206551 0.833838 0.042*
C11 1.0361 (4) 0.5720 (4) 0.1733 (4) 0.0353 (9)
C12 0.5699 (4) 0.1235 (4) 0.3314 (4) 0.0406 (10)
H12 0.638831 0.157971 0.321832 0.049*
C13 0.7317 (5) 0.7601 (4) −0.0551 (4) 0.0501 (12)
H13 0.747657 0.810603 −0.123463 0.060*
C14 1.1016 (4) 0.4370 (4) 0.3494 (4) 0.0450 (11)
H14 1.165146 0.394487 0.402711 0.054*
C15 0.3514 (5) 0.1272 (4) 0.4245 (4) 0.0399 (10)
H15 0.273272 0.163472 0.478704 0.048*
C16 0.6094 (5) 0.7438 (4) −0.0283 (4) 0.0467 (11)
H16 0.541182 0.781887 −0.078147 0.056*
C17 1.0613 (5) 0.6472 (4) 0.0670 (4) 0.0504 (13)
H17 1.146301 0.654664 0.048146 0.060*
C18 1.1332 (4) 0.5060 (4) 0.2505 (4) 0.0456 (11)
H18 1.219982 0.509601 0.233762 0.055*
C19 0.9373 (4) 0.1497 (4) 0.5999 (4) 0.0497 (11)
H19 0.953409 0.176230 0.518666 0.060*
C20 0.8933 (5) 0.0668 (4) 0.8385 (4) 0.0483 (11)
H20 0.877347 0.038601 0.919271 0.058*
C21 0.9661 (5) 0.7073 (5) −0.0065 (4) 0.0519 (12)
H21 0.986551 0.754128 −0.075996 0.062*
C22 0.4812 (7) −0.0336 (4) 0.2814 (5) 0.0676 (17)
H22 0.490113 −0.104517 0.236533 0.081*
C23 1.0148 (5) 0.0091 (4) 0.7713 (5) 0.0576 (13)
H23 1.083009 −0.057440 0.806375 0.069*
C24 1.0369 (5) 0.0491 (5) 0.6516 (5) 0.0679 (16)
H24 1.119620 0.008088 0.604909 0.082*
C25 0.5850 (6) 0.0161 (4) 0.2682 (4) 0.0582 (14)
H25 0.664613 −0.023139 0.216757 0.070*
C26 0.3665 (6) 0.0207 (4) 0.3594 (5) 0.0592 (14)
H26 0.297988 −0.014347 0.368936 0.071*

Source of material

The following compounds 0.0461 g erbium nitrate hexahydrate (0.10 mmol), 0.0180 g 1,10-phenanthroline (0.10 mmol) and 0.0122 g benzoic acid (0.10 mmol) were mixed homogeneously under stirring, then placed in a 25 mL Teflon-lined stainless steel reactor, and finally heated to 120°. Seventy-two hours later, the reactor cooled naturally. Pink crystals were obtained for X-ray single-crystal diffraction test, yield 46% based on Er.

Experimental details

The structure was solved by direct methods with the SHELXS program. All H-atoms were positioned with idealized geometry and refined isotropically (U iso(H) = 1.2 U eq(C) and U iso(H) = 1.2 U eq(N)) using a riding model with C–H = 0.950 Å.

Comment

The four-component dimers of lanthanide complexes composed of lanthanide(III) cations, nitrate, benzoic acid or its derivatives, and 1,10-phenanthroline have been reported with a chemical formula [Ln2(L)4(phen)2(NO3)2] (Ln = lanthanide(III) ions, phen = 1,10-phenanthroline, and L = benzoate or its derivatives) [5], [6], [7], [8], [9], [10], [11]. Also two analogues of erbium complexes (L = 4-acetamidobenzoate [12] and 2-fluorobenzoate [13]) and two isostructures complex (Ln = praseodymium [14] and holmium [15]) have been published elsewhere, respectively. The title complex, with the formula of [Er2(L)4(phen)2(NO3)2] (L = benzoate) has not been reported. The title complex crystallizes in P 1 ‾ located around an inversion center (see the Figure). Consequently the asymmetric unit consists of one Er(III) ion, two benzoates, one phen, and one nitrate. The dimer is made of two asymmetric units linked by four benzoates, which adapt two coordination modes: two of them are in a μ2-k2O:O′ mode while the other two briding ligands use a μ2-k3O,O′:O mode. The distance of the two Er(III) ions is 3.929 Å. The dimers are linked together by weak non-classical hydrogen bonds C10–H10⃛O7, C16–H16⃛O7, and C17–H17⃛O7, and weak π⃛π interactions. All bond lengths are similar to the reported results of its analogues [12, 13].

Corresponding author: Zhang Li, School of Biological and Chemical Engineering, Nanyang Institute of Technology, Nanyang, Henan 473004, 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. Research funding: None declared.

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

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Received: 2022-04-03
Accepted: 2022-06-20
Published Online: 2022-07-06
Published in Print: 2022-10-26

© 2022 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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https://doi.org/10.1515/ncrs-2022-0169
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Articles in the same Issue

  1. Frontmatter
  2. New Crystal Structures
  3. The crystal structure of 3-(1-(2-((5-methylthiophen-2-yl)methylene)hydrazinyl)ethylidene)chroman-2,4-dione, C17H14N2O3S
  4. Crystal structure of chlorido-(η 6-toluene)(5,5′-dimethyl-2,2′-bipyridine-κ2 N,N′)ruthenium(II) hexafluoridophosphate(V) ─ acetone (1/1) C22H26ClN2ORuPF6
  5. Crystal structure of 4-(((2-(3-(1-(3-(3-cyanophenyl)-6-oxopyridazin-1(6H)-yl)ethyl)phenyl) pyrimidin-5-yl)oxy)methyl)-1-methylpiperidin-1-ium chloride monohydrate, C30H33N6O2Cl
  6. The crystal structure of 2-chloro-N-((2-chlorophenyl)carbamoyl)nicotinamide, C13H9Cl2N3O2
  7. Crystal structure of 9-(t-butyl)-3,11-dihydro-6H-pyrazolo [1,5-a]pyrrolo[3′,2′:5,6]pyrido[4,3-d]pyrimidin-6-one hemihydrate, C30H32N10O3
  8. Crystal structure of di-μ2-hydroxido-tetrakis(6-methylpyridine-2-carboxylato-k2 N,O) diiron(III) trihydrate C28H32Fe2N4O13
  9. Crystal structure of catena-poly[qua-(μ2-2-aminoisophthalat-κ3 O,O′:O′′)(1,10-phenanthroline-κ2 N,N′)manganese(II)] C20H15MnN3O5
  10. Crystal structure of poly[(bis(isothiocyano)-bis(μ 2-(E)-N′-(pyridin-4-ylmethylene)isonicotinohydrazide))iron(II) – methanol – 1,4-dioxane (1/2/2), C36H44FeN10O8S2
  11. Crystal structure of (E)-N′-(1-(5-chloro-2-hydroxyphenyl)propylidene)-4-hydroxybenzohydrazide, C16H15ClN2O3
  12. Crystal structure of bis(μ2-benzoato-k2O:O′)-bis(μ2-benzoato-k3O,O′:O′)dinitrato-k2O,O′-bis(phenanthroline-k2 N,N′)dierbium(III), C52H36Er2N6O14
  13. Crystal structure of 4-ethyl-2-{[(4-nitrophenyl)methyl]sulfanyl}-6-oxo-1,6-dihydropyrimidine-5-carbonitrile, C14H12N4O3S
  14. Synthesis and crystal structure of 1-((3R,10S,13R,17S)-10,13-dimethyl-3- (phenylamino)hexadecahydro-1H-cyclopenta[α] phenanthren-17-yl)ethan-1-one, C27H39NO
  15. Crystal structre of 1,4-bis(bromomethyl)-2,3,5,6-tetramethylbenzene, C12H16Br2
  16. Crystal structure of 2-(adamantan-1-yl)-5-(3,5-dinitrophenyl)-1,3,4-oxadiazole, C18H18N4O5
  17. Crystal structure of (E)-N′-benzylidene-4-nitrobenzohydrazide – methanol (1/1), C15H15N3O4
  18. The crystal structure of 3-(2-bromophenyl)-1,5-di-p-tolylpentane-1,5-dione, C25H23BrO2
  19. Crystal structure of catena-poly[(μ 2-4,4′-bipyridine-κ2 N:N′)-bis(4-bromobenzoato-κ1 O)zinc(II)], C24H16Br2N2O4Zn
  20. Crystal structure of 1,1′-(1,2-ethanediyl)bis(pyridin-1-ium) bis(1,2-dicyanoethene-1,2-dithiolato-κ2 S:S)zinc(II), C20H14N6ZnS4
  21. Crystal structure of pentacarbonyl-(μ2-propane-1,3-dithiolato-κ4 S:S,S′:S′)-(diphenyl(o-tolyl)phosphine-κ1 P)diiron (Fe-Fe), C27H23Fe2O5PS2
  22. The crystal structure of the cocrystal 4-hydroxy-3,5-dimethoxybenzoic acid–pyrazine-2-carboxamide(1/1), C14H15N3O6
  23. The crystal structure of dichlorido-bis((RS)-2-(4-chlorophenyl)-2-(1,2,4-triazol-1-ylmethyl)hexanenitrile-κ1 N)zinc(II), C30H34Cl4N8Zn
  24. Crystal structure of the cocrystal 2,4,6-triamino-1,3,5-triazine – 1H-isoindole-1,3(2H)-dione – methanol (1/1/1), C12H15N7O3
  25. The crystal structure of methyl 4-((3,5-di-tert-butyl-4-oxocyclohexa-2,5-dien-1-ylidene)methyl) benzoate, C23H28O3
  26. Crystal structure of (poly[µ2-(1H-pyrazol-1-yl)methyl]-1H-benzotriazole-κ 2 N:N)-(nitrato-κ 2 O:O′) silver(I), C9H8AgN7O3
  27. Crystal structure of tetraaqua-bis[4-(1H-1,2,4-triazol-1-yl)benzoato-k1 N]cadmium(II), C18H20CdN6O8
  28. The crystal structure of diaqua-bis(pyrazolo[1,5-a]pyrimidine-3-carboxylato-κ2N,O)nickel(II) dihydrate, C14H16N6O8Ni
  29. Crystal structure of poly[μ2-aqua-aqua-(μ2-1,3-di(1H-imidazol-1-yl)propane-κ2 N:N′)-(μ2-4,4′-(1H-1,2,4-triazole-3,5-diyl)dibenzoato-κ2 O:O′)-(μ4-4,4′-(1H-1,2,4-triazole-3,5-diyl)dibenzoato-κ5 O,O′:O″:O′″:O′″)dicobalt(II)] – water – dimethylformamide (1/1/1) C44H43N11O12Co2
  30. Crystal structure of N-((Z)-amino(((E)-amino(phenylamino)methylene) amino)methylene)benzenaminium chloride – benzo[f]isoquinolino[3,4-b][1,8]naphthyridine – tetrahydrofurane (1/2/2), C60H54ClN11O2
  31. The crystal structure of Chrysosplenol D, C18H16O8
  32. Crystal structure of poly[deca aqua-bis(μ 4-2-(triazol-1-yl)-benzene-1,3,5-tricarboxylato)- bis(μ 5-2-(triazol-1-yl)-benzene-1,3-dicarboxylato-5-carboxyl acid) pentamanganese(II)] dihydrate, C44H42Mn5N12O36
  33. Synthesis and crystal structure of (E)-1-(4-(((E)-3-(tert-butyl)-2-hydroxybenzylidene)amino)phenyl)ethan-1-one O-methyl oxime, C20H24N2O2
  34. The crystal structure of 4,4′-dichloro-6,6′-dimethoxy-2,2′,3,3′,5,5′- hexanitroazobenzene, C14H6N8O14Cl2
  35. Crystal structure of N 2,N 4-dimesitylpentane-2,4-diamine, C23H34N2
  36. Crystal structure of (1,4,7,10,13,16-hexaoxacyclooctadecane-κ 6O6)potassium(2-methylphenylamino)ethyl-2-methylphenylamide ammoniate (1/3.5), [K(18-crown-6)](o-CH3C6H4)NH(CH2)2N(o-CH3C6H4) 3.5 NH3, C28H53.5KN5.5O6
  37. The crystal structure of N′,N″,2-tris((E)-5-chloro-2-hydroxybenzylidene)hydrazine-1-carbohydrazonhydrazide hydrochloride – methanol (1/3), C25H30Cl4N6O6
  38. Crystal structure of (E)-7-bromo-2-(3,5-dimethoxybenzylidene)-3,4-dihydronaphthalen-1(2H)-one, C19H17BrO3
  39. Crystal structure of (E)-N′-(1-(5-chloro-2-hydroxyphenyl) ethylidene)-4-hydroxybenzohydrazide, C15H13ClN2O3
  40. {2-(((2-aminoethyl)imino)methyl)-6-bromophenolato-κ3 N,N′,O}iron(III) nitrate, C18H20Br2FeN5O5
  41. Crystal structure of 2-(tert-pentyl)anthracene-9,10-dione, C19H18O2
  42. Crystal structure of 5,5′-(1,4-phenylene)bis(1H-imidazol-3-ium) bis(2-(2-(carboxymethyl)phenyl)acetate), C32H30N4O8
  43. Crystal structure of N 2,N 6-bis(2-(((E)-naphthalen-1-ylmethylene)amino)phenyl)pyridine-2,6-dicarboxamide, C41H29N5O2
  44. The crystal structure of 3-amino-1,2,4-triazolium 2,4,5-trinitroimidazolate, C5H5O6N9
  45. Hydrogen bonded dimers in the crystal structure of 2-chloro-N-(phenylcarbamoyl)nicotinamide, C26H20Cl2N6O4
  46. The crystal structure of 4,4′-bipyridine-5,6,7-trihydroxy-2-phenyl-4H-chromen-4-one-water(1/2/2), C40H32N2O12
  47. Crystal structure of N,N'-bis(4-fluoro-salicylaldehyde)-3,6-dioxa-1,8-diaminooctane, C20H22F2N2O4
  48. Crystal structure of 3-(1,3-dinitropropan-2-yl)-4H-chromen-4-one, C12H10N2O6
  49. The crystal structure of (4-(2-bromoethoxy)-phenyl)(phenyl)methanone, C15H13BrO2
  50. Crystal structure of (E)-7-bromo-2-(4-methoxybenzylidene)-3,4-dihydronaphthalen-1(2H)-one, C18H15BrO2
  51. Crystal structure of dichlorido-tetrakis((E)-(RS)-1-(2,4-dichlorophenyl)-4,4-dimethyl-2-(1,2,4-triazol-1-yl)pent-1-en-3-ol-κ 1 N)cadmium(II), C60H68O4N12Cl10Cd
  52. Crystal structure of diaqua-diphenanthroline-κ2 N,N′-bis(μ2-2-carboxy-3,4,5,6-tetrafluorobenzoato-κ2 O:O′)-bis(μ2-tetrafluorophthalato-κ3 O,O′:O′)didysprosium(III) – phenanthroline (1/2), C80H38Dy2F16N8O18
  53. Crystal structure of bis(μ2-2-oxido-2-phenylacetato-κ3 O,O′:O′)-bis(N-oxido-benzamide-κ2 O,O′)-bis(propan-2-olato-κ1 O)dititanium(IV), C36H38N2O12Ti2
  54. Crystal structure of poly[diaqua-(μ2-1H-benzo[d][1,2,3]triazole-5-carboxylato-κ2 O:O′)(μ2-oxalato-κ4O,O:O″,O′″)europium(III)] monohydrate, C9H10N3O9Eu
  55. Crystal structure of bis((N-methyl-2-oxyethyl)amine)-bis(μ 2-N,N,N-tris(2-oxoethyl)amine)-bis(isopropoxy)-bis(μ 3-oxo)tetratitanium(IV)– isopropanol (1/2), C34H76N4O16Ti4
  56. Synthesis and crystal structure of ethyl 4-((4-iodobenzyl)amino)benzoate, C16H16INO2
  57. Crystal structure of (Z)-2-(tert-butyl)-5-((5-(tert- butyl)-2H-pyrrol-2-ylidene)(mesityl)methyl)-1H-pyrrole, C26H34N2
  58. Crystal structure of dimethylammonium poly[μ4-1,1′-(1,4- phenylenebis(methylene))bis(1H-pyrazole-3,5-dicarboxylato-κ6 N,O:O′:N′,O″:O‴) manganese(II)], C22H26MnN6O8
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