Home Physical Sciences Crystal structure of poly-[(μ2-(carboxylatomethyl)((3-nitrophenyl)sulfonyl)amido-κ3N:O:O′)(μ2-4,4′-bipyridine-κ2N:N′) nickel(II)], C18H14NiN4O6S
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Crystal structure of poly-[(μ2-(carboxylatomethyl)((3-nitrophenyl)sulfonyl)amido-κ3N:O:O′)(μ2-4,4′-bipyridine-κ2N:N′) nickel(II)], C18H14NiN4O6S

  • Zheng-Jun Liu EMAIL logo , Xiao-Miao Chen , Jing-Song Cheng , Tao-Li Deng and Lan Qin
Published/Copyright: February 21, 2019

Abstract

C18H14NiN4O6S, trigonal, R3̄ (no. 148), a = 31.014(11) Å, b = 31.014(11) Å, c = 10.125(7) Å, V = 8434(8) Å3, Z = 18, Rgt(F) = 0.0380, wRref(F2) = 0.0941, T = 296(2) K.

CCDC no.: 1503985

The title crystal structure is shown in the figure. Tables 1 and 2 contain details on crystal structure and measurement conditions and a list of the atoms including atomic coordinates and displacement parameters.

Table 1:

Data collection and handling.

Crystal:Green block
Size:0.26 × 0.25 × 0.21 mm
Wavelength:Mo Kα radiation (0.71073 Å)
μ:1.19 mm−1
Diffractometer, scan mode:CCD, φ and ω
θmax, completeness:28.4°, >99%
N(hkl)measured, N(hkl)unique, Rint:17895, 4697, 0.046
Criterion for Iobs, N(hkl)gt:Iobs > 2 σ(Iobs), 3385
N(param)refined:271
Programs:Bruker [1], SHELX [2], [3], Olex2 [4]
Table 2:

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

AtomxyzUiso*/Ueq
Ni10.08130(2)0.38507(2)0.30183(3)0.02756(10)
S10.18734(2)0.45589(2)0.15518(6)0.03231(15)
O10.30621(9)0.49945(10)0.5643(3)0.0795(8)
O20.34202(8)0.57868(9)0.5889(2)0.0738(7)
O30.20460(6)0.48022(7)0.02977(17)0.0475(5)
O40.20257(7)0.42085(6)0.1921(2)0.0483(5)
O50.02357(6)0.40384(6)−0.02796(16)0.0347(4)
O60.03396(6)0.37658(6)0.16340(18)0.0426(5)
N10.31029(9)0.53977(11)0.5402(2)0.0523(6)
N20.12992(7)0.43266(7)0.16831(19)0.0337(5)
N30.29729(7)0.39022(8)0.9094(2)0.0355(5)
N40.12869(7)0.39010(7)0.44477(19)0.0321(4)
C10.27523(9)0.54153(10)0.4478(2)0.0382(6)
C20.26979(11)0.58229(11)0.4457(3)0.0540(8)
H20.2879040.6088590.5027440.065*
C30.23679(13)0.58319(12)0.3571(4)0.0694(10)
H30.2322370.6106370.3552210.083*
C40.21033(11)0.54449(10)0.2712(3)0.0500(7)
H40.1881980.5458170.2116220.060*
C50.21684(8)0.50364(9)0.2741(2)0.0316(5)
C60.24906(8)0.50160(9)0.3649(2)0.0349(6)
H60.2529520.4737960.3698550.042*
C70.10423(9)0.44162(11)0.0608(3)0.0458(7)
H7A0.1180120.439278−0.0231190.055*
H7B0.1089620.4748910.0684880.055*
C80.05012(8)0.40429(8)0.0654(2)0.0278(5)
C90.29295(10)0.37192(10)0.7890(3)0.0455(7)
H90.3129510.3586320.7659520.055*
C100.26046(10)0.37155(10)0.6965(3)0.0455(7)
H100.2589810.3588040.6124500.055*
C110.22997(9)0.39044(9)0.7304(2)0.0335(5)
C120.23376(10)0.40843(11)0.8551(3)0.0448(7)
H120.2137200.4212640.8817580.054*
C130.26746(10)0.40744(11)0.9411(3)0.0446(7)
H130.2693610.4195591.0261880.054*
C140.19494(9)0.39122(9)0.6324(2)0.0319(5)
C150.18187(9)0.42784(10)0.6293(3)0.0397(6)
H150.1949550.4534820.6910060.048*
C160.14956(9)0.42597(9)0.5346(3)0.0375(6)
H160.1417320.4512670.5330270.045*
C170.14134(9)0.35504(9)0.4487(2)0.0374(6)
H170.1270910.3293740.3872260.045*
C180.17387(9)0.35459(9)0.5374(3)0.0380(6)
H180.1819860.3295150.5341660.046*

Source of material

To a 20 mL Teflon-lined reaction vessel was added nickel(II) acetate tetrahydrate (124.4 mg, 0.5 mmol), 3-nitrobenzenesulfonylglycine (H2nbs) (130.1 mg, 0. 5 mmol), 4,4′-bipyridine (4,4′-bipy) (78.1 mg, 0.5 mmol) and 15 mL water. Then the pH of the resulting mixture was adjusted to 7 with 1 mol/L NaOH aqueous solution. After heating at 120 °C for 24 h, the mixture was cooled to room temperature at a rate of 10 °C per hour to give green block crystals.

Experimental details

The structure was solved with the ShelXT [2] structure solution program using intrinsic phasing and refined with the ShelXL [3] refinement package.

Comment

The sulfonylated amino acid has a plurality of coordination sites because it contains both an amino group and a carboxyl group. It can be used to assemble MOFs and CPs [5], [6], [7], [8] which have potential applications in gas adsorption and separations [9], [10], [11], sensors [12], [13], catalysis [14], [15], and fluorescent materials [16].

In this paper, we report the synthesis and the crystal structure of a new nickel(II) complex with 4,4′-bipyridine (4,4′-bipy) and 3-nitrobenzenesulfonylglycine (H2nbs). The asymmetric unit is composed of one Ni(II) ion, one nbs ligand and one 4,4′-bipy ligand. The Ni2+ ion is five-coordinated by two N atoms (N3, N4) from 4,4′-bipy group, two O atoms (O5, O6) and one N atom (N2) from nbs group (Ni1—O, 1.9500(18) ∼ 2.0255(17) Å, Ni1—N, 2.013(2) ∼ 2.168(2) Å). A three-dimensional coordination polymer was formed by Ni—O and Ni—N bonds.

Funding source: Key Project of Guizhou Provincial Education Department

Award Identifier / Grant number: KY[2015]385

Funding source: Youth Science and Technology Talents Growth Project of Guizhou Provincial Education Department

Award Identifier / Grant number: KY[2018]329

Funding source: Platform Project of Anshun University

Award Identifier / Grant number: 2015PT03

Funding statement: The project was supported by Key Project of Guizhou Provincial Education Department (KY[2015]385), Youth Science and Technology Talents Growth Project of Guizhou Provincial Education Department (KY[2018]329) and Platform Project of Anshun University (2015PT03).

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Received: 2018-12-02
Accepted: 2019-01-31
Published Online: 2019-02-21
Published in Print: 2019-03-26

©2019 Zheng-Jun Liu 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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  67. Crystal structure of catena-poly[diaqua-(μ2-1,2-bis(4-pyridinyl)ethyane-κ2N:N′)-(μ2–pyridazine-4,5-dicarboxylato-κ2O:O′)]dizinc(II) dihydrate, C12H12ZnN3O6
  68. The crystal structure of 2-(4-chloro-2,6-dinitrophenyl)-1-(4-chloro)diazene oxide, C12H6Cl2N4O5
  69. Crystal structure of 2-isopropylthioxanthone, C16H14OS
  70. Crystal structure of methyl 2-(4-(3-(1-methyl-1H-pyrazol-4-yl)pyrazolo[1,5-a]pyrimidin-6-yl)phenyl)acetate, C19H17N5O2
  71. Crystal structure of 4,4-dimethyl-2-(trifluoromethyl)-4,5-dihydro-1H-imidazole, C6H9F3N2
  72. Crystal structure of N-methylanilinium 5,7-dihydroxy-4-oxo-2-phenyl-4H-chromene-8-sulfonate monohydrate, C22H21NO8S
  73. Crystal structure of methyl 4-acetoxybenzoate, C10H10O4
  74. Crystal structure of catena-poly[(bis(μ-1,1′-[(5-methoxy-2,4,6-trimethyl-1,3-phenylene)bis(methylene)]bis(1H-1,2,4-triazole)-κ2N:N′)-bis(isothiocyanato-κN)manganese(II)], C34H40MnN14O2S2
  75. Crystal structure of N-(2-methylphenyl)(propan-2-yloxy)carbothioamide, C11H15NOS
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