Startseite Naturwissenschaften Crystal structure of hexakis(μ2-azido-κ2N:N)-diazido-κ1N-tetrakis(phenanthroline-κ2N,N′)tetrazinc(II), C48H32N32Zn4
Artikel Open Access

Crystal structure of hexakis(μ2-azido-κ2N:N)-diazido-κ1N-tetrakis(phenanthroline-κ2N,N′)tetrazinc(II), C48H32N32Zn4

  • Yu-Quan Feng ORCID logo EMAIL logo , Zhi-Guo Zhong und Zi-Long Yue
Veröffentlicht/Copyright: 9. Oktober 2019

Abstract

C48H32N32Zn4, triclinic, P1̄ (no. 2), a = 9.9928(14) Å, b = 10.1374(14) Å, c = 14.2362(19) Å, α = 71.710(2)°, β = 76.166(2)°, γ = 71.086(2)°, V = 1280.1(3) Å3, Z = 1, Rgt(F) = 0.0314, wRref(F2) = 0.0795, T = 296(2) K.

CCDC no.: 1951372

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:Yellow block
Size:0.29 × 0.25 × 0.20 mm
Wavelength:Mo Kα radiation (0.71073 Å)
μ:1.93 mm−1
Diffractometer, scan mode:Bruker APEX-II, φ and ω
θmax, completeness:26.0°, 99%
N(hkl)measured, N(hkl)unique, Rint:8227, 4969, 0.021
Criterion for Iobs, N(hkl)gt:Iobs > 2 σ(Iobs), 3848
N(param)refined:379
Programs:Bruker [1], Olex2 [2], SHELX [3]
Table 2:

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

AtomxyzUiso*/Ueq
Zn10.96883(3)0.48546(3)0.39409(2)0.03393(10)
Zn20.88633(3)0.73656(3)0.19268(2)0.03761(11)
N11.1150(2)0.5437(2)0.45028(17)0.0394(5)
N21.2159(3)0.5871(2)0.40522(19)0.0414(6)
N31.3122(3)0.6298(3)0.3629(3)0.0736(9)
N40.8220(2)0.6963(2)0.34560(17)0.0373(5)
N50.7053(3)0.7486(2)0.38436(18)0.0402(6)
N60.5956(3)0.7995(3)0.4215(2)0.0673(8)
N71.1003(2)0.2713(2)0.39573(16)0.0330(5)
N80.8249(2)0.3800(2)0.37051(17)0.0347(5)
N91.0572(2)0.5552(2)0.23774(18)0.0398(6)
N101.1254(3)0.4710(3)0.18963(19)0.0458(6)
N111.1915(4)0.3893(3)0.1455(2)0.0845(11)
N120.8074(3)0.6455(3)0.1233(2)0.0552(7)
N130.6897(3)0.6693(3)0.1126(2)0.0553(7)
N140.5763(4)0.6887(5)0.0986(3)0.1084(14)
N150.7298(2)0.9507(2)0.16269(17)0.0398(6)
N161.0149(2)0.8784(2)0.14230(16)0.0355(5)
C11.2365(3)0.2204(3)0.4061(2)0.0421(7)
H11.2821(3)0.2812(3)0.4151(2)0.0505(8)*
C21.3152(3)0.0802(3)0.4041(2)0.0489(8)
H21.4111(3)0.0483(3)0.4121(2)0.0587(9)*
C31.2506(3)−0.0093(3)0.3904(2)0.0464(7)
H31.3021(3)−0.1033(3)0.3886(2)0.0557(9)*
C41.1062(3)0.0401(3)0.37888(19)0.0368(6)
C51.0357(3)0.1840(3)0.38149(18)0.0310(6)
C60.8880(3)0.2409(3)0.36952(19)0.0316(6)
C70.8151(3)0.1526(3)0.3572(2)0.0391(6)
C80.8895(3)0.0064(3)0.3575(2)0.0452(7)
H80.8406(3)−0.0535(3)0.3511(2)0.0543(9)*
C91.0275(3)−0.0461(3)0.3669(2)0.0450(7)
H91.0735(3)−0.1414(3)0.3654(2)0.0539(9)*
C100.6716(3)0.2133(3)0.3461(2)0.0512(8)
H100.6186(3)0.1577(3)0.3388(2)0.0615(9)*
C110.6094(3)0.3530(4)0.3460(3)0.0557(8)
H110.5140(3)0.3948(4)0.3373(3)0.0668(10)*
C120.6888(3)0.4329(3)0.3588(2)0.0470(7)
H120.6445(3)0.5288(3)0.3593(2)0.0564(9)*
C130.5884(3)0.9844(3)0.1731(2)0.0498(8)
H130.5437(3)0.9103(3)0.1969(2)0.0597(9)*
C140.5045(3)1.1257(4)0.1500(3)0.0586(9)
H140.4055(3)1.1450(4)0.1576(3)0.0703(11)*
C150.5667(4)1.2352(4)0.1163(2)0.0561(9)
H150.5111(4)1.3303(4)0.1003(2)0.0674(10)*
C160.7156(3)1.2047(3)0.1058(2)0.0459(7)
C170.7924(3)1.0595(3)0.1297(2)0.0375(6)
C180.9458(3)1.0205(3)0.12060(19)0.0359(6)
C191.0153(3)1.1295(3)0.0917(2)0.0429(7)
C200.9337(4)1.2765(3)0.0690(2)0.0540(8)
H200.9801(4)1.3491(3)0.0497(2)0.0648(10)*
C210.7913(4)1.3119(3)0.0750(2)0.0579(9)
H210.7407(4)1.4088(3)0.0588(2)0.0695(11)*
C221.1637(3)1.0852(3)0.0869(2)0.0512(8)
H221.2150(3)1.1536(3)0.0687(2)0.0614(9)*
C231.2336(3)0.9424(4)0.1088(2)0.0511(8)
H231.3326(3)0.9124(4)0.1049(2)0.0614(9)*
C241.1549(3)0.8419(3)0.1369(2)0.0420(7)
H241.2034(3)0.7443(3)0.1527(2)0.0504(8)*

Source of material

The mixture of Zn(NO3)2 ⋅ 6H2O (0.20 g), 1,10-phenanthroline (C12H8N2, 0.16 g), NaN3 (0.10 g) and H2O (3.0 mL) was transferred into 50 mL Teflon-lined stainless steel vessels and heated at 160 °C for 5 days. After cooling to room temperature, the yellow block crystals were isolated, washed with distilled water and dried at room temperature.

Experimental details

H atoms were positioned geometrically and refined using a riding model, with C—H = 0.93 Å, with Uiso(H) = 1.2 times Ueq(C).

Comment

A large number of metal coordination compounds containing various metal cations and organic ligands have been obtained with different dimensional structures. Currently, linking metal cations and organic ligands to build coordination compounds has become a popular synthetic strategy [4]. Polydentate ligands, such as N3 and NCS, can act as either bridging or chelating ligands to construct desired metal-organic coordination compounds [4], [5], [6]. As a part of an ongoing study [6], [7] we have synthesized a tetra-nuclear Zn2+ coordination compound formulated [Zn4(C12H8N2)4(N3)8](1) containing two kinds of ligands.

Single crystal X-ray diffraction indicated that 1 belongs to the triclinic system with the space group P1̄. The molecular structural unit of 1 contains four Zn2+ cations, four C12H8N2 ligands and eightN3anions as shown in the figure. Within the title complex Zn1 is six-coordinated by six N atoms from one C12H8N2 ligand and four N atoms from four N3 ligands. Zn2 cation is five-coordinated by five N atoms from one C12H8N2 ligand and three N atoms from three N3 ligands. The bond distances Zn—N, N—N and the bond angles of N—Zn—N are in the ranges of 1.966(3)–2.209(2) Å, 1.129(3)–1.196(3) Å and 76.53(8)–168.68(9)°, respectively. These above mentioned bond distances and angles are all in their normal ranges. They can be compared with those previously reported compounds [8]. By means of such connected modes, a tetra-nuclear coordination compound was generated. The distances of Zn⋯Zn are 3.251 Å and 3.338 Å. It is worth noting that the eight N3ligands exhibited two types of coordination fashions: six N3ligands as bridged ligands linked to two Zn2+ cations (Zn1 and Zn2) and two N3ligands as terminal ligands connected to Zn2. In addition, C—H⋯N hydrogen bonds are found in the packing structure of 1.

Award Identifier / Grant number: 21601095

Funding statement: This work was financially supported by the National Natural Science Foundation of China (no. 21601095).

References

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Received: 2019-07-06
Accepted: 2019-09-19
Published Online: 2019-10-09
Published in Print: 2019-12-18

©2019 Yu-Quan Feng et al., published by De Gruyter, Berlin/Boston

This work is licensed under the Creative Commons Attribution 4.0 Public License.

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  57. Crystal structure of octa(4-chlorobenzyl)-dichlorido-bis(μ2-methanolato)-bis(μ3-oxo)-tetratin(IV), C58H54Cl10O4Sn4
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  60. Crystal structure of 4-benzyl-1-oxo-N-phenethyl-1H-[1,4]oxazino [4,3-b]indazole-3-carboxamide, C26H21N3O3
  61. Crystal structure of bis{(N-[(5-chloro-2-oxidophenyl)methylidene]-2-hydroxybenzenecarbohydrazonato)-dioxo-molybdenum(VI)}(μ2-4,4′-bipyridine), C38H26Cl2Mo2N6O10
  62. Crystal structure of dichlorido-octamethyl-bis(μ3-oxido)-bis(μ2-2-(phenylamino)ethanolato-κ2O:O)tetratin(IV), C24H44Cl2N2O4Sn4
  63. The crystal structure of 1-(2-(2-(imidazo[1,5-a]pyridine-4-ium)ethoxy)ethyl)-imidazo[1,5-a]pyridine-4-ium bis(hexafluorophosphate) — acetonitrile (1/1), C18H20ON4F12P2
  64. Crystal structure of cyclo[tetra(μ2-cyanido)-tetracyanido-bis(1,4,7,10-tetraazacyclododecane-κ4N,N′,N′′,N′′′)dinickel(II)dipalladium(II)] hexahydrate, C24H52N16Ni2O6Pd2
  65. Crystal structure of (dimethyl sulfoxide)-dioxido-[2-hydroxy-N′-(4-oxo-4-phenylbutan-2-ylidene)benzohydrazidato κ3N,O,O′]molybdenum(VI), C19H20MoN2O6S
  66. Crystal structure of bis(acetylacetonato-κ2O,O′)-(ethanolamine-κ2N,O)copper(II), C14H25CuNO5
  67. Crystal structure of chlorido-diphenyl-(isopropyl(propyl)carbamodithioato-κ2S,S′)tin(IV), C19H24ClNS2Sn
  68. The crystal structure of bis(imidazole-1-yl)methane monohydrate, C7H10N4O
  69. The crystal structure of bis(4-nitroimidazole-1-1yl)methane, C7H6N6O4
  70. Crystal structure of di(naphthalen-2-yl)sulfane, C20H14S
  71. Crystal structure of 3-acetyl-6-bromo-4-hydroxy-2H-chromen-2-one, C11H7BrO4
  72. Crystal structure of N′2,N′6-bis((E)-1-(pyrazin-2-yl)ethylidene)pyridine-2,6-dicarbohydrazide — methanol (1/2), C21H25N9O4
  73. The crystal structure of 3-nitro-4-(p-tolylamino)-2H-chromen-2-one, C16H12N2O4
  74. The crystal structure of 1,2-bis((4-methoxyphenyl)ethynyl)benzene, C24H18O2
  75. Crystal structure of a low-temperature (100 K) polymorph of catena-poly[(μ2-4,4′-bipyridine-κ2N,N′)-bis(O,O′-diethyldithiophosphato-κ1S)zinc(II)], C18H28N2O4P2S4Zn
  76. The pseudosymmetric low temperature polymorph of catena-poly[(μ2-4,4′-bipyridyl-κN,N′)-bis(O,O′-diethyldithiophosphato-κS)-cadmium(II)], {C18H28CdN2O4P2S4}n
  77. Crystal structure of 3-iodophthalic acid, C8H5IO4
  78. The crystal structure of tert-butyl (tert-butoxy(oxo)methyl)(5-bromo-2-fluorophenyl)carbamate, C16H21BrFNO4
  79. The crystal structure of bis(μ2-5,7-dichloroquinolin-8-olato-κ3N,O:O)-tetrakis(5,7-dichloroquinolin-8-olato-κ2N,O)bis(methanol-κ1O)dieuropium(III) — toluene (1/1), C63H39Cl12Eu2N6O8
  80. Crystal structure of dichlorido-(N′-(1-(3-ethylpyrazin-2-yl)ethylidene)-4-methoxybenzohydrazide-κ3N,N′,O)cadmium(II), C16H18N4O2Cl2Cd
  81. A redetermination of the crystal structure of catena-poly[(bis(O,O′-isopropyl dithiophosphato-κ2S,S′)-(μ2-1,2-bis(3-pyridylmethylene)hydrazine-κ2N,N′)cadmium(II)], {C24H38CdN4O4P2S4}n
Heruntergeladen am 9.12.2025 von https://www.degruyterbrill.com/document/doi/10.1515/ncrs-2019-0473/html
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