Home Physical Sciences Crystal structure of poly-[(μ2(carboxylatomethyl)((3-nitrophenyl)sulfonyl)amido-κ3N: O:O′)(μ2-4,4′-bipyridine-κ2N:N′)copper(II)], C18H14CuN4O6S
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Crystal structure of poly-[(μ2(carboxylatomethyl)((3-nitrophenyl)sulfonyl)amido-κ3N: O:O′)(μ2-4,4′-bipyridine-κ2N:N′)copper(II)], C18H14CuN4O6S

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

Abstract

C18H14CuN4O6S, trigonal, R3̄ (no. 148), a = 31.125(7) Å, b = 31.125(3) Å, c = 10.133(2) Å, V = 8501(3) Å3, Z = 18, Rgt(F) = 0.0346, wRref(F2) = 0.0900, T = 296(2) K.

CCDC no.: 1509569

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:Blue block
Size:0.26 × 0.22 × 0.21 mm
Wavelength:Mo Kα radiation (0.71073 Å)
μ:1.31 mm−1
Diffractometer, scan mode:CCD, φ and ω
θmax, completeness:28.4°, >99%
N(hkl)measured, N(hkl)unique, Rint:18075, 4720, 0.033
Criterion for Iobs, N(hkl)gt:Iobs > 2 σ(Iobs), 3698
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
Cu10.91869(2)0.61493(2)0.69823(2)0.02795(9)
S10.81264(2)0.54406(2)0.84485(5)0.02849(13)
O10.96602(5)0.62350(6)0.83687(16)0.0390(4)
O20.97650(5)0.59615(6)1.02793(14)0.0314(3)
O30.79534(6)0.51970(6)0.97045(16)0.0429(4)
O40.79736(6)0.57902(6)0.80803(19)0.0448(4)
O50.69391(9)0.50036(9)0.4349(2)0.0736(7)
O60.65803(7)0.42132(8)0.4113(2)0.0671(6)
N10.87009(6)0.56722(7)0.83157(17)0.0304(4)
N20.68978(8)0.46048(9)0.4591(2)0.0477(5)
N30.70273(7)0.60979(7)0.08981(18)0.0323(4)
N40.87125(6)0.60984(7)0.55560(17)0.0290(4)
C10.94988(7)0.59577(7)0.9350(2)0.0249(4)
C20.89581(8)0.55827(10)0.9397(2)0.0418(6)
H2A0.8912070.5251650.9320070.050*
H2B0.8820300.5605591.0235200.050*
C30.78311(7)0.49621(8)0.7256(2)0.0283(4)
C40.75084(8)0.49837(8)0.6359(2)0.0309(5)
H40.7468490.5260170.6313020.037*
C50.72479(8)0.45846(9)0.5534(2)0.0357(5)
C60.73014(10)0.41752(10)0.5557(3)0.0493(7)
H60.7118020.3909650.4991730.059*
C70.76320(12)0.41652(11)0.6432(3)0.0606(8)
H70.7678700.3892570.6450650.073*
C80.78947(10)0.45543(10)0.7281(3)0.0469(6)
H80.8116480.4542780.7874550.056*
C90.70693(9)0.62805(9)0.2118(2)0.0414(6)
H90.6868190.6410290.2354100.050*
C100.73959(9)0.62848(9)0.3036(2)0.0414(6)
H100.7412590.6415020.3873200.050*
C110.77000(8)0.60947(8)0.2712(2)0.0290(4)
C120.76639(9)0.59151(10)0.1445(2)0.0409(6)
H120.7864510.5788390.1177420.049*
C130.73267(9)0.59261(10)0.0584(2)0.0417(6)
H130.7308460.580599−0.0267140.050*
C140.80483(8)0.60855(8)0.3679(2)0.0293(4)
C150.82601(9)0.64540(9)0.4625(2)0.0357(5)
H150.8181410.6705460.4650050.043*
C160.85852(9)0.64486(9)0.5522(2)0.0348(5)
H160.8725130.6702690.6141220.042*
C170.85045(8)0.57388(8)0.4650(2)0.0340(5)
H170.8583340.5487370.4663860.041*
C180.81814(8)0.57204(8)0.3702(2)0.0351(5)
H180.8052660.5466530.3079990.042*

Source of material

Copper(II) acetate monohydrate (99.8 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 was added to a 20 mL Teflon-lined reaction vessel. 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, it was cooled to room temperature at a rate of 10 °C per hour to give blue 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 using least squares minimisation.

Comment

Metal-organic frameworks (MOFs) are a class of organic-inorganic hybrid materials. In recent years, it has gained great attention due to their diverse structures and rich physical and chemical properties, such as electricity, light, and magnetism etc., and potential applications in gas adsorption/storage and separation [5], [6], [7], [8], identification and sensing [9], [10], [11], and heterogeneous catalysis [12], [13]. The sulfonylated amino acid compound which has some coordination sites can be used to assemble metal organic frameworks and coordination polymers [14], [15], [16], [17].

In this paper, the synthesis and crystal structure of a new copper(II) complex with 3-nitrobenzenesulfonylglycine (H2nbs) and 4,4′-bipyridine (4,4′-bipy) is reported. The asymmetric unit is composed of one independent Cu(II) ion, one nbs ligand and one 4,4′-bipy ligand. The crystallographically unique Cu2+ ion of the title complex is five-coordinated (see the figure) by two N atoms (N3, N4) from 4,4′-bipy group, two O atoms (O1, O2) and one N atom (N1) from nbs group (Cu1—O, 1.9549(15) ∼ 2.0309(14) Å, Cu1—N, 2.0150(17) ∼ 2.1705(18) Å). A three-dimensional network was formed by Cu—O and Cu—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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  64. The crystal structure of dichloroido(1,3-bis(2,6-dimethyl-phenyl)-1H-3l4-imidazol-2-yl)(2-methyl-4,5-dihydrooxazol-κN)palladium(IV)-water (1/1), C23H29Cl2N3O2Pd
  65. Crystal structure of catena-poly[dibromido-{μ2-1,5-dimethyl-2-phenyl-4-((pyridin-4-ylmethylene)amino)-1,2-dihydro-3H-pyrazol-3-one-κ2N:O}zinc(II)], C34H32Br4N8O2Zn2
  66. Crystal structure of diaqua-dichlorido-bis(μ2-2-(((1,5-dimethyl-3-oxo-2-phenyl-2,3-dihydro-1H-pyrazol-4-yl)imino)methyl)phenolato-κ4O:O,N,O′)dicobalt(II), C36H36Cl2N6O6Co2
  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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