Startseite The crystal structure of [(2,2′-bipyridine-κ2 N,N)-bis(6-phenylpyridine-2-carboxylato- κ2 N,O)nickel(II)] monohydrate, C34H26N4O5Ni
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The crystal structure of [(2,2′-bipyridine-κ2 N,N)-bis(6-phenylpyridine-2-carboxylato- κ2 N,O)nickel(II)] monohydrate, C34H26N4O5Ni

  • Zhou Tingting ORCID logo und Cao Zhen EMAIL logo
Veröffentlicht/Copyright: 12. September 2022

Abstract

C34H26N4O5Ni, monoclinic, C2/c (no. 15), a = 29.3459(13) Å, b = 10.2867(4) Å, c = 19.8780(9) Å, β = 107.243(5)°, V = 5730.9(4) Å3, Z = 8, Rgt (F) = 0.0326, wRref (F 2) = 0.0817, T = 200K.

CCDC no.: 2203647

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: Colourless block
Size: 0.14 × 0.11 × 0.10 mm
Wavelength: Mo Kα radiation (0.71073 Å)
μ: 0.73 mm−1
Diffractometer, scan mode: SuperNova, ω
θ max, completeness: 25.0°, >99%
N(hkl)measured, N(hkl)unique, R int: 13553, 5050, 0.029
Criterion for I obs, N(hkl)gt: I obs > 2 σ(I obs), 4373
N(param)refined: 400
Programs: Bruker [1], Olex2 [2], SHELX [3], Diamond [4]
Table 2:

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

Atom x y z U iso*/U eq
Ni1 0.37812 (2) 0.42744 (2) 0.31050 (2) 0.01678 (9)
O1 0.36054 (5) 0.49693 (16) 0.49901 (8) 0.0351 (4)
O2 0.38738 (5) 0.51119 (14) 0.40550 (7) 0.0251 (3)
O3 0.36154 (5) 0.59180 (13) 0.25273 (8) 0.0240 (3)
O4 0.39089 (5) 0.77336 (13) 0.22049 (8) 0.0282 (3)
N1 0.30634 (5) 0.40977 (14) 0.32063 (8) 0.0171 (4)
N2 0.44915 (5) 0.50927 (15) 0.32391 (8) 0.0179 (4)
N3 0.38758 (5) 0.23826 (15) 0.35524 (9) 0.0192 (4)
N4 0.37223 (5) 0.31111 (16) 0.22302 (8) 0.0195 (4)
C1 0.26496 (7) 0.36150 (18) 0.27780 (10) 0.0200 (4)
C2 0.22850 (7) 0.3218 (2) 0.30462 (12) 0.0269 (5)
H2 0.200866 0.285318 0.274779 0.032*
C3 0.23317 (7) 0.3362 (2) 0.37491 (12) 0.0317 (5)
H3 0.208928 0.309696 0.393148 0.038*
C4 0.27436 (7) 0.3906 (2) 0.41802 (12) 0.0292 (5)
H4 0.278101 0.403825 0.465635 0.035*
C5 0.31003 (7) 0.42513 (18) 0.38916 (10) 0.0201 (4)
C6 0.35639 (7) 0.4827 (2) 0.43571 (11) 0.0238 (5)
C7 0.25687 (7) 0.36060 (19) 0.20070 (11) 0.0217 (4)
C8 0.23635 (8) 0.2545 (2) 0.15954 (12) 0.0337 (5)
H8 0.230389 0.178792 0.181035 0.040*
C9 0.22473 (9) 0.2605 (2) 0.08695 (13) 0.0391 (6)
H9 0.211395 0.188565 0.059926 0.047*
C10 0.23281 (8) 0.3724 (2) 0.05465 (12) 0.0355 (6)
H10 0.224872 0.376449 0.005796 0.043*
C11 0.25276 (8) 0.4790 (2) 0.09484 (12) 0.0340 (5)
H11 0.258002 0.555131 0.072986 0.041*
C12 0.26491 (7) 0.4729 (2) 0.16724 (11) 0.0258 (5)
H12 0.278644 0.544817 0.193978 0.031*
C13 0.37075 (7) 0.3531 (2) 0.15890 (10) 0.0252 (5)
H13 0.370348 0.442177 0.150840 0.030*
C14 0.36981 (8) 0.2699 (2) 0.10407 (12) 0.0341 (6)
H14 0.368987 0.302254 0.060035 0.041*
C15 0.37011 (8) 0.1381 (2) 0.11597 (12) 0.0360 (6)
H15 0.369466 0.080002 0.079854 0.043*
C16 0.37137 (8) 0.0927 (2) 0.18162 (12) 0.0300 (5)
H16 0.371559 0.003919 0.190436 0.036*
C17 0.37235 (7) 0.18171 (19) 0.23436 (10) 0.0201 (4)
C18 0.37564 (6) 0.1422 (2) 0.30681 (10) 0.0204 (4)
C19 0.36774 (8) 0.0157 (2) 0.32513 (12) 0.0310 (5)
H19 0.359627 −0.049051 0.290996 0.037*
C20 0.37205 (8) −0.0125 (2) 0.39419 (13) 0.0381 (6)
H20 0.366040 −0.096108 0.407257 0.046*
C21 0.38532 (8) 0.0840 (2) 0.44368 (13) 0.0355 (6)
H21 0.388757 0.066594 0.490839 0.043*
C22 0.39350 (7) 0.2072 (2) 0.42252 (11) 0.0266 (5)
H22 0.403594 0.271438 0.456605 0.032*
C24 0.39499 (7) 0.67046 (19) 0.25470 (10) 0.0202 (4)
C25 0.44351 (6) 0.63412 (19) 0.30278 (10) 0.0194 (4)
C26 0.47900 (7) 0.7262 (2) 0.32388 (12) 0.0299 (5)
H26 0.473912 0.811046 0.307144 0.036*
C27 0.52231 (8) 0.6901 (2) 0.37041 (13) 0.0351 (6)
H27 0.546590 0.750798 0.386568 0.042*
C28 0.52884 (7) 0.5631 (2) 0.39232 (12) 0.0300 (5)
H28 0.557696 0.536946 0.423668 0.036*
C29 0.49216 (7) 0.4735 (2) 0.36752 (10) 0.0212 (4)
C30 0.50000 (7) 0.3348 (2) 0.38690 (11) 0.0238 (5)
C31 0.52156 (8) 0.2984 (2) 0.45652 (13) 0.0358 (6)
H31 0.530867 0.361368 0.491477 0.043*
C32 0.52911 (9) 0.1682 (3) 0.47355 (15) 0.0489 (7)
H32 0.542910 0.143620 0.520184 0.059*
C33 0.51618 (9) 0.0743 (3) 0.42137 (18) 0.0525 (8)
H33 0.521383 −0.013085 0.433109 0.063*
C34 0.49568 (8) 0.1099 (2) 0.35224 (15) 0.0429 (6)
H34 0.487361 0.046892 0.317151 0.051*
C35 0.48754 (7) 0.2399 (2) 0.33535 (13) 0.0294 (5)
H35 0.473498 0.263874 0.288680 0.035*
O5 0.36041 (7) 0.7513 (2) 0.07137 (10) 0.0522 (5)
H5A 0.367315 0.744953 0.115915 0.078*
H5B 0.360572 0.673382 0.057214 0.078*

Source of material

To 0.2488 g (1.0 mmol) Ni(CH3COO)2·4H2O was added a solution of 0.1992 g (1.0 mmol) 6-phenylpyridine-2-carboxylic acid and 0.040 g (1.0 mmol) NaOH in 20 mL ethanol-distilled water (v:v = 1:1) with stirring. After 30 min, 0.1562 g (1.0 mmol) 2,2′-bipyridine was added. Then the solution was heated at 75 °C for 6 h. After cooled to room temperature, the solution was filtered and volatiled slowly at room temperature. The block crystals of the title compound were obtained after 30 days. Elemental analysis (%) calcd. for C34H26N4O5Ni: C, 64.83; H, 4.13; N, 8.90. Found (%): C, 64.99; H, 4.36; N, 8.69.

Experimental details

The hydrogen atoms were positioned geometrically (C–H = 0.93 Å and O–H = 0.85 Å). Their U iso values were set to 1.2Ueq or 1.5Ueq of the parent atoms.

Comment

The studies on the properties and structures of metal complexes have been one of the priorities of coordination chemists. Because they showed wide potential application for example [58]. Tai’s research team reported the structures of Mn(II), Co(II), Cu(II), Zn(II) and Pb(II) complexes using 6-phenylpyridine-2-carboxylate ligand [9], [10], [11], [12], [13], [14], [15]. In view of the above studies, in this work, we reported a Ni(II) complex, using 6-phenylpyridine-2-carboxylic acid, Ni(CH3COO)2·4H2O.

The molecular structure of the title complex is shown in the figure. The Ni(II) complex is made up of a Ni(II) ion, two 6-phenylpyridine-2-carboxylate ligands, one 2,2′-bipyridine ligand and one lattice water molecule. The title complex is for example isomorphous to the related manganese(II) complex [9]. The 6-phenylpyridine-2-carboxylate ligands adopt a bidentate coordination mode. The Ni(II) ion is six-coordinated with two N atoms (N1, N2) and two O atoms (O2, O3) from two different 6-phenylpyridine-2-carboxylate ligands, two N atoms (N3, N4) from one 2,2′-bipyridine ligand, respectively. Which forms a distorted octahedral coordination polyhedron. The sum of bond angles of O2–Ni1–N1 (79.35(6)°), N2–Ni1–O2 (82.11(6)°), N2–Ni1–N4 (99.42(6)°) and N4–Ni1–N1 (100.74(6)°) is 361.62°, and N3–Ni1–O3 is 169.88(6)°), indicating that the center Ni(II) ion is in the same plane with N1,O2,N2,O4 atoms and N3, O3 atoms are at the axial position. The bond lengths of Ni1–N1, Ni1–O2, Ni1–N2, Ni1–N4, Ni1–O3 and Ni1–N3 are 2.1822(15), 2.0193(13), 2.1896(15), 2.0755(16), 2.0206(13) and 2.1233(16) Å, respectively, which are consistent with those reported in the literature [5]. The complexes are interconnected by intermolecular O–H⃛O hydrogen bonds including oxygen atoms of lattice water molecules and the carboxyl oxygen atoms of 6-phenylpyridine-2-carboxylate ligand to form chain architecture.


Corresponding author: Cao Zhen, College of Chemistry and Chemical Engineering, Weifang University, Weifang, Shandong 261061, P. R. China, E-mail:

Funding source: Shandong Provincial Natural Science Foundation

Award Identifier / Grant number: ZR2019BEM017

Funding source: Weifang University Doctoral Research Funding

Award Identifier / Grant number: 2019BS007

Award Identifier / Grant number: 21171132

Award Identifier / Grant number: ZR2014BL003

Award Identifier / Grant number: J14LC01

Funding source: 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 Shandong Provincial Natural Science Foundation (ZR2019BEM017); Weifang University Doctoral Research Funding (2019BS007); National Natural Science Foundation of China (No. 21171132), the Natural Science Foundation of Shandong (ZR2014BL003), the Project of Shandong Province Higher Educational Science and Technology Program (J14LC01) and Science Foundation of Weifang (2020ZJ1054).

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

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Received: 2022-07-16
Accepted: 2022-08-26
Published Online: 2022-09-12
Published in Print: 2022-12-16

© 2022 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

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  2. New Crystal Structures
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  29. Crystal structure of E-2-chloro-N′-(1-(5-chloro-2-hydroxyphenyl)propylidene)benzohydrazide, C16H14Cl2N2O2
  30. Crystal structure of 3-(adamantan-1-yl)-4-methyl-5-{[(4-nitrophenyl)methyl]sulfanyl}-4H-1,2,4-triazole, C20H24N4O2S
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  36. [2,2′-{Ethane-1,2-diylbis[(azanylylidene)methanylylidene]}bis(3-bromo-2-hydroxyphenyl)]iron(III) nitrate, C20H12Br2CuN2O2
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  38. Synthesis and crystal structure of 2-(2-oxo-2-(thiophen-2-yl)ethyl)-4H-chromen-4-one, C15H10O3S
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  45. Crystal structure of dichlorido-tetra((E)-(RS)-1-(2,4-dichlorophenyl)-4,4-dimethyl-2-(1,2,4-triazol-1-yl)pent-1-en-3-ol-κ1 N)zinc(II), C60H68O4N12Cl10Zn
  46. The crystal structure of 4-(2-bromoethoxy)-2-hydroxybenzaldehyde, C9H9BrO3
  47. The crystal structure of 5-azido-1-methyl-4-nitroimidazole, C4H4O2N6
  48. Crystal structure of dibromido-tetra((E)-(RS)-1-(2,4-dichlorophenyl)-4,4-dimethyl-2-(1,2,4-triazol-1-yl)pent-1-en-3-ol-κ 1 N)zinc(II), C60H68O4N12Br2Cl8Zn
  49. Crystal structure of tetrasodium-bis(μ 2-oxido)-hexafluoro-didioxo-molybdenum(V), Na2(Mo2O4F6)
  50. Crystal structure of (E)-N′-(2-chloro-6-hydroxybenzylidene)-4- hydroxybenzohydrazide-water (1/1), C14H13Cl1N2O4
  51. Crystal structure of (E)-N-(4-morpholinophenyl)-1-(quinolin-2-yl)methanimine, C20H19N3O
  52. The crystal structure of catena-poly[(1,10-phenanthroline-κ2 N,N′)-(μ3-2-hydroxybenzene-1,3-dicarboxylato-κ5 O,O′:O″,O‴:O‴)cadmium(II)], C20H12CdN2O5
  53. The crystal structure of 2,6-di-tert-butyl-4-(4-(methylthio)benzylidene)cyclohexa-2,5-dien-1-one, C22H28OS
  54. La3.65Mg30Sb1.07 as a disordered derivative of Th2Ni17-type structure
  55. Crystal structure of (E)-N-(4-morpholinophenyl)-1-(quinoxalin-2-yl)methanimine, C19H18N4O
  56. The crystal structure of 2,2′-(1,2-phenylenebis(methylene))bis(1,3-dimethylisothiouronium) bromide, C14H24Br2N4S2
  57. Crystal structure of tetraaqua-bis[4-(1H-1,2,4-triazol-1-yl)benzoato-κ1 N]zinc(II), C18H20ZnN6O8
  58. Crystal structure of bis(tricarbonyl)-{(S)-(tert-butoxycarbonyl)(1-methoxy-1-oxo-3-sulfido-k2 S:S′-propan-2-yl)amido-k2N:N′}diiron(I) (Fe—Fe), C15H15Fe2NO10S
  59. Crystal structure of (E)-3-((4-chlorophenyl)thio)-4-hydroxypent-3-en-2-one, C11H11ClO2S
  60. The crystal structure of (E)-3′,6′-bis(diethylamino)-2-((5-(diethylamino)-2-hydroxybenzylidene)amino)spiro[isoindoline-1,9′-xanthen]-3-one, C39H45N5O3
  61. The crystal structure of 2-(4-methoxynaphthalen-1-yl)-4H-chromen-4-one, C20H14O3
  62. The crystal structure of trans-dichlorido-(ethylenediamine-κ 2 N,N′)-bis(triphenylphosphine-κ 1 P)ruthenium(II), C38H38Cl2N2P2Ru
  63. The double polymeric chain of catena-poly[(μ2-6-bromopyridine-3-carboxylato-κ2 O,O′) (6-bromopyridine-3-carboxylato-κ2 O,O′) (μ2-1,2-bis(4-pyridyl)ethylene-κ2 N:N′)cobalt(II)], C24H16CoBr2N4O4
  64. The crystal structure of tert-butyl 2-(4-(12-bromo [2.2]paracyclophanyl)carbamoyl)pyrrolidine-1-carboxylate, C26H31BrN2O3
  65. The crystal structure of (Z)-2-(2,3-dimethoxybenzylidene)naphtho[1,2-b]furan-3(2H)-one, C21H16O4
  66. Crystal structure of 2-hydroxy-1-tosylindolin-3-yl- 2-naphthoate, C26H21N1S1O5
  67. The crystal structure of 1-methyl-N-(1-methyl-1H-imidazole-2-carbonyl)-1H-imidazole-2-carboxamide, C10H11N5O2
  68. The crystal structure of (E)-2-((5-bromo-2-hydroxybenzylidene)amino)-3′,6′-bis(ethylamino)-2′, 7′-dimethylspiro[isoindoline-1,9′-xanthen]-3-one, C33H31BrN4O3
  69. The crystal structure of dimethanol-5,15-diphenylporphyrin-21,23-diido-κ4 N,Nʹ,Nʺ,Nʹʺ-manganese(III) trans-dicyanido-bis(acetylacetonato-κ2O,Oʹ)ruthenium(III), C46H42N6O6RuMn
  70. Crystal structure of 1,4,8,11-tetraazacyclotetradecane-1,8-diium bis(3,5-dicarboxybenzoate), C28H36N4O12
  71. Bifurcated halogen bonds in the crystal structure of 2,2′-bi(1,8-naphthyridine)—1,4-diiodotetrafluorobenzene (1/1), C22H10F4I2N4
Heruntergeladen am 8.9.2025 von https://www.degruyterbrill.com/document/doi/10.1515/ncrs-2022-0361/html
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