Home Crystal structure of (diaqua-bis(phenanthroline-K 2 N,N′)-tetrakis(m 2-3,4,5,6-tetrafluorophthalato-K 4 O,O:O′:O″;K 2 O:O′)dierbium (III) phenanthroline (1/2), C80H38Er2F16N8O18
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Crystal structure of (diaqua-bis(phenanthroline-K 2 N,N′)-tetrakis(m 2-3,4,5,6-tetrafluorophthalato-K 4 O,O:O′:O″;K 2 O:O′)dierbium (III) phenanthroline (1/2), C80H38Er2F16N8O18

  • Jun-Ya Song , Xiao-Yu Zhang ORCID logo EMAIL logo , Chun-Li Zhang , Bei-Bei Zhao , Shi-Jie Huang and Xinfang Liu EMAIL logo
Published/Copyright: March 27, 2023
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Zeitschrift für Kristallographie - New Crystal Structures
From the journal Zeitschrift für Kristallographie - New Crystal Structures Volume 238 Issue 3

Abstract

C80H38Er2F16N8O18, triclinic, P 1 ‾ (no. 2), a = 11.4228(4) Å, b = 12.6712(3) Å, c = 13.2663(4) Å, α = 102.660(2)°, β = 98.047(3)°, γ = 105.509(3)°, V = 1764.54(10) Å3, Z = 1, R gt(F) = 0.0311, wR ref (F 2) = 0.0668, T = 293(2) K.

CCDC no.: 2235105

The asymmetric unit of 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.

Figure: The molecular structure of the title compound, showing the atom numbering scheme. Displacement ellipsoids are shown at the 30% probability level.
Figure:

The molecular structure of the title compound, showing the atom numbering scheme. Displacement ellipsoids are shown at the 30% probability level.

Table 1:

Data collection and handling.

Crystal: Colourless block
Size: 0.20 × 0.19 × 0.18 mm
Wavelength: Mo Kα radiation (0.71073 Å)
μ: 2.49 mm−1
Diffractometer, scan mode: SuperNova, ω
θ max, completeness: 29.1°, >99%
N(hkl)measured, N(hkl)unique, R int: 15,821, 8127, 0.034
Criterion for I obs, N(hkl)gt: I obs > 2 σ(I obs), 7495
N(param)refined: 561
Programs: CrysAlis Pro [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 0.58494 (2) 0.16248 (2) 0.55111 (2) 0.01820 (5)
F1 0.5363 (2) 0.19806 (18) 0.00720 (16) 0.0467 (6)
F2 0.2935 (2) 0.12846 (17) −0.08053 (16) 0.0440 (5)
F3 0.1286 (2) −0.0091 (2) 0.00034 (18) 0.0541 (6)
F4 0.20538 (19) −0.07264 (16) 0.17039 (16) 0.0411 (5)
F5 1.0644 (2) 0.24678 (17) 0.56698 (19) 0.0500 (6)
F6 1.1730 (2) 0.18881 (19) 0.73143 (19) 0.0528 (6)
F7 1.0458 (2) 0.00672 (18) 0.79144 (16) 0.0429 (5)
F8 0.8218 (2) −0.12321 (16) 0.68203 (17) 0.0419 (5)
O1 0.6936 (2) 0.2511 (2) 0.2149 (2) 0.0474 (7)
O2 0.6749 (2) 0.0697 (2) 0.2140 (2) 0.0397 (6)
H2 0.7401 0.0965 0.2585 0.060*
O3 0.5078 (2) 0.11221 (16) 0.36582 (16) 0.0247 (5)
O4 0.4227 (2) −0.07749 (16) 0.30500 (17) 0.0278 (5)
O5 0.6461 (2) −0.17597 (16) 0.49578 (19) 0.0323 (6)
O6 0.61447 (19) −0.01466 (16) 0.48870 (17) 0.0217 (5)
O7 0.8569 (2) 0.1082 (2) 0.36340 (19) 0.0392 (6)
O8 0.7554 (2) 0.19275 (16) 0.46982 (17) 0.0251 (5)
O9 0.7677 (2) 0.24310 (18) 0.68284 (18) 0.0297 (5)
H9A 0.7512 0.2435 0.7452 0.044*
H9B 0.7995 0.3151 0.6872 0.044*
N1 0.6284 (2) 0.35821 (19) 0.5296 (2) 0.0231 (6)
N2 0.5334 (3) 0.3014 (2) 0.6946 (2) 0.0253 (6)
C1 0.4992 (3) 0.1074 (2) 0.1432 (2) 0.0235 (7)
C2 0.4139 (3) 0.0375 (2) 0.1865 (2) 0.0221 (7)
C3 0.2922 (3) −0.0037 (3) 0.1341 (3) 0.0291 (7)
C4 0.2498 (3) 0.0265 (3) 0.0447 (3) 0.0325 (8)
C5 0.3326 (3) 0.0963 (3) 0.0043 (3) 0.0301 (8)
C6 0.4564 (3) 0.1335 (3) 0.0517 (3) 0.0269 (7)
C7 0.6341 (3) 0.1526 (3) 0.1950 (3) 0.0306 (8)
C8 0.4535 (3) 0.0226 (2) 0.2951 (2) 0.0215 (6)
C9 0.8190 (3) −0.0048 (2) 0.5654 (2) 0.0210 (6)
C10 0.8824 (3) 0.0925 (2) 0.5377 (2) 0.0228 (7)
C11 1.0020 (3) 0.1529 (3) 0.5930 (3) 0.0288 (7)
C12 1.0584 (3) 0.1255 (3) 0.6776 (3) 0.0325 (8)
C13 0.9959 (3) 0.0321 (3) 0.7062 (3) 0.0287 (7)
C14 0.8785 (3) −0.0331 (3) 0.6489 (3) 0.0263 (7)
C15 0.6865 (3) −0.0721 (2) 0.5130 (2) 0.0199 (6)
C16 0.8259 (3) 0.1341 (2) 0.4496 (3) 0.0235 (7)
C17 0.4821 (3) 0.2743 (3) 0.7726 (3) 0.0332 (8)
H17 0.4619 0.1990 0.7754 0.040*
C18 0.4567 (4) 0.3530 (3) 0.8508 (3) 0.0421 (10)
H18 0.4203 0.3300 0.9040 0.051*
C19 0.4853 (4) 0.4634 (3) 0.8487 (3) 0.0414 (9)
H19 0.4684 0.5165 0.9004 0.050*
C20 0.5697 (4) 0.6106 (3) 0.7587 (3) 0.0446 (10)
H20 0.5548 0.6663 0.8092 0.054*
C21 0.6181 (4) 0.6391 (3) 0.6791 (3) 0.0404 (9)
H21 0.6374 0.7141 0.6756 0.049*
C22 0.6894 (3) 0.5814 (3) 0.5127 (3) 0.0372 (9)
H22 0.7103 0.6556 0.5068 0.045*
C23 0.7055 (3) 0.4974 (3) 0.4383 (3) 0.0368 (9)
H23 0.7375 0.5134 0.3807 0.044*
C24 0.6737 (3) 0.3865 (3) 0.4489 (3) 0.0297 (8)
H24 0.6847 0.3297 0.3969 0.036*
C25 0.6124 (3) 0.4420 (2) 0.6046 (3) 0.0227 (7)
C26 0.6408 (3) 0.5552 (2) 0.5987 (3) 0.0306 (8)
C27 0.5400 (3) 0.4964 (3) 0.7688 (3) 0.0318 (8)
C28 0.5616 (3) 0.4121 (2) 0.6914 (2) 0.0227 (7)
N3 0.9074 (3) 0.4650 (2) 0.7305 (2) 0.0395 (7)
N4 0.8259 (3) 0.3905 (2) 0.8968 (3) 0.0411 (8)
C29 0.7941 (4) 0.3579 (4) 0.9799 (3) 0.0509 (11)
H29 0.7723 0.2807 0.9755 0.061*
C30 0.7914 (4) 0.4322 (4) 1.0737 (4) 0.0599 (12)
H30 0.7689 0.4050 1.1302 0.072*
C31 0.8224 (4) 0.5450 (4) 1.0805 (4) 0.0581 (12)
H31 0.8207 0.5962 1.1419 0.070*
C32 0.8908 (4) 0.7022 (4) 0.9971 (4) 0.0609 (13)
H32 0.8864 0.7551 1.0561 0.073*
C33 0.9282 (4) 0.7372 (3) 0.9159 (4) 0.0584 (12)
H33 0.9484 0.8142 0.9191 0.070*
C34 0.9848 (4) 0.6949 (4) 0.7406 (4) 0.0543 (12)
H34 1.0086 0.7716 0.7425 0.065*
C35 0.9951 (4) 0.6181 (4) 0.6583 (4) 0.0592 (12)
H35 1.0295 0.6412 0.6042 0.071*
C36 0.9537 (4) 0.5027 (4) 0.6543 (3) 0.0523 (11)
H36 0.9588 0.4500 0.5954 0.063*
C37 0.9010 (3) 0.5426 (3) 0.8171 (3) 0.0323 (8)
C38 0.9380 (4) 0.6597 (3) 0.8245 (3) 0.0425 (9)
C39 0.8572 (4) 0.5842 (3) 0.9947 (3) 0.0443 (10)
C40 0.8593 (3) 0.5036 (3) 0.9042 (3) 0.0342 (8)

1 Source of materials

A mixture of Er(NO3)3⋅6H2O (0.0923 g, 0.2 mmol), 3,4,5,6- tetrafluorophthalic acid (0.054 g, 0.2 mmol) and phenanthroline (35.7 mg, 0.15 mmol) were dissolved in 8 mL of deionized water. The mixture was sealed in a 25 mL Teflon-lined steel autoclave after ultrasound treatment for 15 min and heated at 120 °C for 72 h. The mixture was cooled to room temperature at a rate of 2 °C/h, and colorless block crystals were isolated by filtration, washed with distilled water and dried in air (CCDC number 2235105).

2 Experimental details

Using Olex2 [2], the structure was solved with the ShelXT [3] structure solution program and refined with the ShelXL [4] refinement package. The carbon bound hydrogen atoms were placed in calculated positions and refined using a riding model on attached atoms.

3 Comment

In recent decades, a large number of Er(III) complexes have attracted considerable attentions due to their structural diversity and potential applications in many areas [5], [6], [7], [8]. Er(III)–MOFs can be constructed from Er(III) ions and carboxylate and nitrogen-containing ligands. Among rod N-donor ligands, 1,10-phenanthroline (1,10–Phen) has been extensively used in the preparation of Er complexes [5], [6], [7]. However, tetrafluorophthalic acid (H2TFPA), as a common derivative of phthalic acid, is rarely used in the assembly process [8]. In this work, a binuclear Er(III) complex was constructed with TFPA and 1,10–Phen as mixed ligands. The asymmetric unit contains one Er(III), two tetrafluorophthalate (HTFPA−), one coordinated water molecule, one coordinated 1,10–Phen, and one free 1,10–Phen molecule (see Figure). Er1 is nine-coordinated by two N atoms (N1, N2) of phen ligand, one O atom (O9) from coordinated water molecule, two O atoms (O3, O4#1, #1: 1 − x, −y, 1 − z) from two HTFPA− ligands and four O atoms (O6, O8, O5#1 and O6#1) from two TFPA2− ligands. The Er–N bond lengths are 2.484(2) and 2.543(2) Å and the Er–O bond lengths are in the range of 2.339(2)–2.686(2) Å, respectively. Two HTFPA− and two TFPA2− ligands adopt bis-monodentate and bis-bidentate bridging modes, respectively, to link neighboring Er(III) ions into a nuclear {Er2} unit.

Corresponding author: Xiao-Yu Zhang, College of Food and Bioengineering, Henan University of Science and Technology, Luoyang, Henan 471022, P. R. China, E-mail: ; and Xinfang Liu, College of Chemistry and Chemical Engineering, Henan Key Laboratory of Function-Oriented 6 Porous Materials, Luoyang Normal University, Luoyang, 471934, P. R. China, E-mail:

Funding source: Training Program for Young Cadre Teachers of Higher Education Institutions in Henan Province

Award Identifier / Grant number: 2018GGJS128

Funding source: Science and Technology Development Project in Henan Province

Award Identifier / Grant number: 172101410037

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

  2. Research funding: This work was supported by the Training Program for Young Cadre Teachers of Higher Education Institutions in Henan Province (No. 2018GGJS128) and Science and Technology Development Project in Henan Province (No. 172101410037).

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

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Received: 2023-01-10
Accepted: 2023-03-14
Published Online: 2023-03-27
Published in Print: 2023-06-27

© 2023 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-2023-0023
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Articles in the same Issue

  1. Frontmatter
  2. New Crystal Structures
  3. Crystal structure of phenyl(3,3-dichloro-1,3-dihydro-2H-pyrrolo[2,3-b]pyridin-2-one)methanone, C7H4Cl2N2O
  4. Crystal structure of poly[diaqua-bis(μ 2-1,4-diaminobutane-N:N′)cobalt(II)] dichloride, C8H28Cl2CoN4O2
  5. Synthesis and crystal structure of (4aR,7S)-7-hydroxy-7-isopropyl-1,1-dimethyldecahydro-2H,6H-8a,4a-(epoxymethano)phenanthren-12-one, C20H32O3
  6. The crystal structure of 1-(2-chlorobenzyl)-3-(3,5-dichlorophenyl)urea, C14H11Cl3N2O
  7. Crystal structure of tetrapropylammonium-1,3,5-thiadiazole-5-amido-2-carbamate – 1,2,4-thiadiazole-3,5-diamine – water (1/1/1), C17H37N9O3S2
  8. Tetrabutylammonium 1,3,5-thiadiazole-5-amido-2-carbamate—1,2,4-thiadiazole-3,5-diamine— water (1/1/1), C21H45N9O3S2
  9. The crystal structure of ((E)-2,4-dichloro-6-(((2-hydroxy-5-nitrophenyl)imino)methyl)phenolato-κ 3 N,O,O′)tris(pyridine-κN)manganese(II), C28H21Cl2MnN5O4
  10. The crystal structure of aqua-bis{2-bromo-6-((2-(2-phenylacetyl)hydrazineylidene)methyl)phenolato-κ3 N,O,O′}-dimethylformamide-κ1 O-erbium(III) chloride – dimethylformamide – water (1/2/1), C39H49N7O9Br2ClEr
  11. Crystal structure of (diaqua-bis(phenanthroline-K 2 N,N′)-tetrakis(m 2-3,4,5,6-tetrafluorophthalato-K 4 O,O:O′:O″;K 2 O:O′)dierbium (III) phenanthroline (1/2), C80H38Er2F16N8O18
  12. Crystal structure of (E)-7-methoxy-2-(4-methoxy-2-(trifluoromethyl)benzylidene)-3,4-dihydronaphthalen-1(2H)-one, C20H17F3O3
  13. The crystal structure of 4–(4,4,5,5–tetramethyl–1,3,2–dioxaborolan–2–yl)morpholine, C10H20BNO3
  14. The crystal structure of catena–poly[aqua(1-naphthoato-κ 2 O,O′)-(μ-1-naphthoato-κ 4 O:O,O′:O′)lead(II)], C22H16O5Pb
  15. The crystal structure of 1-(4-chlorophenyl)-3-cycloheptylurea, C14H19ClN2O
  16. The crystal structure of 4-(pyren-1-yl)butyl-4-nitrobenzoate, C27H21NO4
  17. Crystal structure of cyclo-(bis(µ2-3,3′-(1H-imidazole-3-ium-1,3-diyl)dipropionato-κ4 O,O′:O″,O″′)-dinitrato-κ2 O,O′-tetraoxido-diuranium(VI) C18H22N6O18U2
  18. The crystal structure of catena-[nitrato-κ 2 O,O′-(μ 3-3-iodobenzene-1,2-dicarboxylato-κ 4 O:O′:O″,O‴)-(2,2′:6′,2″-terpyridine-κ 3 N,N′,N″)lanthanum(III)], C23H14IN4O7La
  19. Redetermination of crystal structure of [bis(pyridin-2-ylmethyl)amine-κ 3 N,Nʹ,Nʺ]chloridopalladium(II) chloride monohydrate
  20. Crystal structure of catena-poly[triaqua-[bis(m2-4-(1H-1,2,4-triazol-1-yl)benzoato-k2O:O')-(4-(1H-1,2,4-triazol-1-yl)benzoato-k1O)-praseodymium (III) monohydrate], C27H26N9O10Pr
  21. Crystal structure of trans-diaqua-bis(methyl methylcarbamohydrazonothioato-κ2 N,N′) nickel(II) iodide semihydrate, C6H22N6O2NiS2I2·0.5H2O
  22. The crystal structure of 2-(2-fluoro-4-methyl-5-((2,2,2-trifluoroethyl)thio)phenyl)isoindolin-1-one, C17H13F4NOS
  23. The crystal structure of di-μ-1-naphthylacetato-κ 3 O,O′:O;κ 3 O:O,O′-bis[(1-naphthylacetato-κ 2 O,O′)(2,2′-bipyridine-κ 2 N,N′)lead(II)] monohydrate, C68H54N4O9Pb2
  24. Crystal structure of tetrapropylammonium guanidinium 4,4′-sulfonyldibenzoate monohydrate, C27H44N4O7S
  25. Crystal structure of bis(tetrapropylammonium) terephthalate – 1-(diaminomethylene)thiourea – water (1/2/4) C18H40N5O4S
  26. Crystal structure of (E)-7-fluoro-2-(4-morpholinobenzylidene)-3,4-dihydronaphthalen-1(2H)-one, C21H20FNO2
  27. The crystal structure of poly[diaqua-bis(μ 3-5-bromobenzene-1,3-dicarboxylato-κ 3 O,O,O′)-(μ 2-1,3-bis-(4-pyridyl)-propane-κ 2 N,N′)-dizinc(II))] – 5-bromobenzene-1,3-dicarboxylic acid [2/1], C37H29Br3N2O14Zn2
  28. The crystal structure of 2-bromo-1,3-phenylene bis(4-methylbenzenesulfonate), C20H17BrO6S2
  29. Crystal structure of europium dichromium icosaaluminum, EuCr2Al20
  30. The crystal structure of N′1,N′3-di((E)-benzylidene) isophthalohydrazide dihydrate, C 22 H 22 N 4 O 4
  31. Crystal structure of 7α,11α-dihydroxy-15-oxo-ent-kauran-16-en-19,6β-olide, C20H26O5
  32. Crystal structure of 4-chloro-N′-[(1E)-pyridin-3-ylmethylidene]benzohydrazide, C13H10ClN3O
  33. The crystal structure of (Z)-3-(1-(2-((E)-4-isopropylbenzylidene)hydrazinyl)ethylidene) chroman-2,4-dione, C21H20N2O3
  34. Crystal structure of E-7-fluoro-2-(2-(trifluoromethyl)benzylidene)-3,4-dihydronaphthalen-1(2H)-one, C18H12F4O
  35. Crystal structure of bis(6-aminopyridine-2-carboxylato–k2O,N)-bis(N,N-dimethylformamide-k1 O)zinc(II), C18H24N6O6Zn
  36. Crystal structure of 5-(adamantan-1-yl)-3-[(4-{[2-(trifluoromethyl)phenyl]-methyl}piperazin-1-yl)methyl]-1,3,4-oxadiazole-2(3H)-thione, C25H31F3N4OS
  37. Crystal structure of tetrapropylammonium bicarbonate–1-(diaminomethylene)thiourea – water (2/2/1), C30H72N10O7S2
  38. Crystal structure of tris(2,2′-bipyridine-κ2 N,N′)iron(II) triiodide – dichloromethane (2/1), C61H50Cl2Fe2I12N12
  39. Crystal structure of 2-amino-3-[2-(1,3,3-trimethyl-1,3-dihydro-indol-2-ylidene)-ethylideneamino]-but-2-enedinitrile, C17H17N5
  40. The crystal structure of 1-(2-chlorophenyl)-3-cycloheptylurea, C14H19ClN2O
  41. Crystal structure of potassium bis(pentaselenido-κ 2 Se 1,Se 5)palladate(II), K2[Pd(Se5)2]
  42. The crystal structure of 5,10-bis(2-methoxyethyl)-5,10-dihydro-[1,2,3,4]tetrathiocino[5,6-b:8, 7-b′]diindole, C22H22N2O2S4
  43. The crystal structure of 4-(4-iodophenyl)-5H-1,2,3-dithiazole-5-thione, C8H4INS3
  44. Crystal structure of bis{μ2-(4-acetyl-phenoxy)acetato-κ2 O:O′}-bis{μ2-(4-acetyl-phenoxy)acetato-κ3 O,O′:O)- bis{(4-acetyl-phenoxy)acetato-κ2 O,O′}-bis(phenanthrolin-κ2 N,N′)didysprosium(III) tetrahydrate, C84H78N4O28Dy2
  45. Crystal structure of Eu2Pd3.37(1)Zn13.63(1)
  46. Crystal structure of 2-methoxy-4-(methoxy-carbonyl)phenyl 2-chloro-4-fluorobenzoate, C16H12ClFO5
  47. Crystal structure of catena-poly[bis(μ2-dicyanamide-κ2 N:N′)-bis(4-vinylpyridine-κN)-copper(II)], C18H14CuN8
  48. The crystal structure of iguratimod-dimethylformamide (1/1), C17H14N2O6S·C3H7NO
  49. Synthesis and crystal structure of 1-((3R,10S,13S,17S)-10,13-dimethyl-3-(m-tolylamino)hexadecahydro-1H-cyclopenta[α]phenanthren-17-yl)ethan-1-one, C28H41NO
  50. The crystal structure of diaqua-bis(4-bromo-2-formylphenoxy)zinc(II), C14H12Br2O6Zn
  51. The crystal structure of tetra(1-ethylimidazole-κ 1 N)-[μ 4-imidazole-4,5-dicarboxylato-κ 4 O, N, O′, N′]-trioxido-divanadium, C25H33N10O7V2
  52. The crystal structure of (E)-N′-(1-(4-fluorophenyl)propylidene)-2-hydroxybenzohydrazide, C16H15FN2O2
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