Home 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
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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

  • Bin Cai ORCID logo EMAIL logo and Yuning Meng
Published/Copyright: March 16, 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

C23H14IN4O7La, triclinic, P 1 ‾ (no. 2), a = 8.2438(3) Å, b = 12.3786(5) Å, c = 12.6230(5) Å, α = 111.802(1)°, β = 91.144(1)°, γ = 100.6470(10)°, V = 1169.86(8) Å3, Z = 2, R gt(F) = 0.0313, wR ref(F 2) = 0.1051, T = 296 K.

CCDC no.: 2246341

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: Colourless block
Size: 0.25 × 0.20 × 0.15 mm
Wavelength: Mo Kα radiation (0.71073 Å)
μ: 3.20 mm−1
Diffractometer, scan mode: φ and ω
θ max, completeness: 25.0°, >99%
N(hkl) measured, N(hkl) unique, R int: 28,225, 4123, 0.052
Criterion for I obs, N(hkl) gt: I obs > 2 σ(I obs), 3535
N(param) refined: 325
Programs: Bruker [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
C1 0.4184 (7) 0.6668 (6) 0.2866 (5) 0.0339 (14)
H1 0.471366 0.720550 0.357220 0.041*
C2 0.2912 (7) 0.6960 (6) 0.2386 (6) 0.0385 (15)
H2 0.255416 0.766018 0.277999 0.046*
C3 0.2181 (8) 0.6218 (6) 0.1332 (6) 0.0427 (16)
H3 0.134074 0.641176 0.097883 0.051*
C4 0.2707 (7) 0.5167 (6) 0.0792 (5) 0.0408 (16)
H4 0.222502 0.464385 0.006707 0.049*
C5 0.3952 (7) 0.4901 (5) 0.1334 (5) 0.0317 (14)
C6 0.4517 (7) 0.3767 (5) 0.0797 (5) 0.0311 (13)
C7 0.3598 (9) 0.2852 (6) −0.0151 (6) 0.0509 (19)
H7 0.262806 0.294611 −0.046345 0.061*
C8 0.4139 (9) 0.1813 (7) −0.0617 (6) 0.061 (2)
H8 0.352463 0.118190 −0.123854 0.073*
C9 0.5593 (9) 0.1707 (6) −0.0161 (6) 0.0526 (19)
H9 0.597574 0.100315 −0.047283 0.063*
C10 0.6485 (7) 0.2644 (5) 0.0759 (5) 0.0334 (14)
C11 0.8129 (7) 0.2616 (5) 0.1231 (5) 0.0331 (14)
C12 0.8972 (9) 0.1741 (7) 0.0634 (7) 0.060 (2)
H12 0.850296 0.114823 −0.006305 0.072*
C13 1.0528 (10) 0.1761 (7) 0.1091 (7) 0.068 (3)
H13 1.110703 0.117448 0.070951 0.082*
C14 1.1192 (8) 0.2643 (6) 0.2096 (6) 0.0478 (18)
H14 1.223650 0.267667 0.241457 0.057*
C15 1.0306 (7) 0.3477 (5) 0.2630 (5) 0.0376 (15)
H15 1.077449 0.408149 0.332131 0.045*
C16 0.5014 (6) 0.6860 (5) 0.5815 (5) 0.0239 (12)
C17 0.4106 (7) 0.7848 (5) 0.5848 (4) 0.0236 (12)
C18 0.4925 (7) 0.9028 (5) 0.6277 (5) 0.0323 (14)
C19 0.4116 (8) 0.9930 (5) 0.6333 (6) 0.0455 (17)
H19 0.468649 1.071721 0.664711 0.055*
C20 0.2478 (8) 0.9666 (6) 0.5926 (6) 0.0454 (17)
H20 0.193053 1.027137 0.596525 0.054*
C21 0.1653 (7) 0.8497 (5) 0.5460 (5) 0.0373 (15)
H21 0.054968 0.831487 0.516583 0.045*
C22 0.2430 (6) 0.7590 (5) 0.5419 (5) 0.0251 (12)
C23 0.1478 (7) 0.6325 (5) 0.4868 (5) 0.0251 (12)
I1 0.74624 (5) 0.95341 (4) 0.68699 (4) 0.04903 (17)
La1 0.72448 (4) 0.52213 (3) 0.34616 (3) 0.02114 (13)
N1 0.4705 (6) 0.5647 (4) 0.2372 (4) 0.0308 (11)
N2 0.5949 (6) 0.3674 (4) 0.1253 (4) 0.0274 (11)
N3 0.8796 (6) 0.3482 (4) 0.2223 (4) 0.0315 (11)
N4 0.8609 (6) 0.7189 (4) 0.2585 (4) 0.0316 (12)
O1 0.5876 (5) 0.6507 (3) 0.4998 (3) 0.0316 (9)
O2 0.4874 (4) 0.6512 (3) 0.6624 (3) 0.0271 (9)
O3 0.2016 (4) 0.5524 (3) 0.5053 (3) 0.0286 (9)
O4 0.0159 (5) 0.6146 (4) 0.4242 (4) 0.0347 (10)
O5 0.7996 (5) 0.7445 (4) 0.3518 (4) 0.0374 (10)
O6 0.8524 (5) 0.6091 (4) 0.1995 (3) 0.0378 (10)
O7 0.9275 (6) 0.7936 (4) 0.2232 (4) 0.0512 (12)

1 Source of materials

The educts 0.433 g lanthanum hexahydrate (1 mmol), 0.292 g (1 mmol) 3-iodobenzene-1,2-dicarboxylic acid, 0.233 g 2,2′:6′,2″-terpyridine (1 mmol), and 0.080 g NaOH (2 mmol) were mixed with 8 mL H2O, then added to a 25 mL Teflon-lined stainless steel autoclave at 413 K for 72 h. Many colourless block crystals were separated, washed with distilled water and anhydrous ethanol, then dried in air. Yield: 66% (based on 3-iodobenzene-1,2-dicarboxylic acid).

2 Experimental details

The structure was solved by direct methods with the Shelxs-2018 program. All H-atoms from C and N atoms were positioned with idealized geometry (U iso(H) = 1.2U eq(C)) using a riding model with C–H = 0.93 Å.

3 Comment

Although benzenedicarboxylic acid, including benzene-1,2-, 1,3- and 1,4-dicarboxylic acids and 2,2′:6′,2″-terpyridine or their derivatives have been used as co-ligands to construct some lanthanide complexes [5], [6], [7], [8], [9], [10], [11], to the best of our knowledge, there has not been reported any result of lanthanide complex based on 3-iodobenzene-1,2-dicarboxylic acid and 2,2′:6′,2″-terpyridine.

As shown in the figure, the asymmetrical unit is made of one La(III) cation, one 3-iodobenzene-1,2-dicarboxylate anion, one 2,2′:6′,2″-terpyridine and one nitrate. The La(III) cation is nine-coordinated by four oxygen atoms (O1, O2#A, O3#A and O4#B, code #A: 1 − x, 1 − y, 1 − z; code #B: 1 + x, y, z) from three completely deprotonated μ 3-iodobenzene-1,2-dicarboxylate anions, two oxygen atoms from one μ 2-nitrate (O5 and O6), and three nitrogen atoms (N1, N2 and N3) from one 2,2′:6′,2″-terpyridine. The neighbouring La(III) cations are linked by μ 3-iodobenzene-1,2-dicarboxylate anions to generate chain structure, further connected by nonclassical hydrogen bonds C4–H4H7⃛O6, C7–H7⃛O7 and C20–H20H7⃛O5, with HH7⃛A distances 2.460, 2.440 and 2.643 Å, respectively. All of the bond lengths are similar to the reported results [5], [6], [7], [8], [9], [10], [11].

Corresponding author: Bin Cai, College of Materials and Chemical Engineering, Henan University of Urban Construction, Pingdingshan 467036, Henan, 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. Conflict of interest statement: The authors declare no conflicts of interest regarding this article.

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Received: 2023-01-22
Accepted: 2023-03-05
Published Online: 2023-03-16
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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  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
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  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
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  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
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https://doi.org/10.1515/ncrs-2023-0036
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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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