Home The crystal structure of tetrakis(1,3,5-triaza-7-phosphatricyclo[3.3.1.13,7]decane-κP)silver(I) chloride dihydrate, C24H60AgClN12O6P4
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The crystal structure of tetrakis(1,3,5-triaza-7-phosphatricyclo[3.3.1.13,7]decane-κP)silver(I) chloride dihydrate, C24H60AgClN12O6P4

  • Runé Oosthuizen , Alice Brink and Gertruida J. S. Venter EMAIL logo
Published/Copyright: August 11, 2017

Abstract

C24H60AgClN12O6P4, tetragonal, P42/nmc (no. 137), a = 14.1874(3) Å, c = 9.8721(3) Å, V = 1987.08(1) Å3, Z = 2, Rgt(F) = 0.0148, wRref(F2) = 0.0417, T = 100 K.

CCDC no.: 1565199

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

Table 1

Data collection and handling.

Crystal:Colourless cuboid
Size:0.52 × 0.36 × 0.26 mm
Wavelength:Mo Kα radiation (0.71073 Å)
μ:7.9 cm−1
Diffractometer, scan mode:Bruker APEX-II, φ and ω
2θmax, completeness:56°, >99%
N(hkl)measured, N(hkl)unique, Rint:55782, 1291, 0.024
Criterion for Iobs, N(hkl)gt:Iobs > 2 σ(Iobs), 1214
N(param)refined:72
Programs:Bruker programs [1], SIR2014 [2], DIAMOND [3], ORTEP [4], SHELX [5]
Table 2

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

AtomxyzUiso*/Ueq
C10.65153(8)0.41564(7)0.50996(11)0.0189(2)
H1A0.59170.41760.45840.023*
H1B0.64750.36290.57530.023*
C20.750.50994(10)0.30730(16)0.0196(3)
H2Aa0.80640.5150.24870.023*
H2Ba0.69360.5150.24870.023*
C30.66570(8)0.58639(7)0.49257(11)0.0220(2)
H3A0.66340.64510.54660.026*
H3B0.60890.5850.43440.026*
C40.750.50462(11)0.66677(16)0.0213(3)
H4A0.750.44790.72510.026*
H4B0.750.56050.72680.026*
N10.750.58877(9)0.40522(13)0.0201(3)
N20.66285(7)0.50518(6)0.58538(9)0.01967(19)
P10.750.39341(3)0.39143(4)0.01630(9)
Cl0.750.250.750.01964(15)
Ag10.750.250.250.01466(7)
O10.49539(6)0.50461(6)0.750.0269(3)
H10.5449(13)0.5058(12)0.7069(18)0.049(5)*
O20.750.750.23494(17)0.0230(3)
H20.750.7045(17)0.287(2)0.045(7)*
  1. aOccupancy: 0.5.

Source of materials

1,3,5-Triaza-7-phosphaadamantane (PTA) (0.1023 g, 0.6510 mmol) and silver chloride (0.0235 g, 0.1642 mmol) were dissolved in acetonitrile (10 cm3) and heated under reflux overnight. The mixture was filtered and the filtrate was left to crystallize. Colourless crystals suitable for X-ray diffraction were obtained in 85.2% yield (0.488 g).

Experimental details

The aliphatic H atoms were placed in geometrically idealized positions and constrained to ride on their parent atoms with C—H = 0.99 Å and Uiso(H) = 1.2 Ueq(C). H atoms at the water molecules were refined isotropically.

Comment

The complex obtained is a water soluble four-coordinate silver complex with chloride counterions. The known cytotoxicity and cell malignity of silver and silver nanoparticles suggests that this compound may be a candidate for anticancer development [6]. Many variants of silver complexes have been developed and proved to demonstrate excellent antibacterial and antifungal properties [7], [8], [9], [10]. 1,3,5-Triaza-7-phosphaadamantane (PTA) was selected as the ligand for this complex due to its ability to solubilize transition metal complexes [11], allowing for the introduction into the blood circulatory system as aqueous solubility is a key parameter to help determine rate and extent of drug absorption [12]. Adamantane complexes have also seen considerable success in aqueous phase and biphasic homogenous catalysis; 1,3,5-triaza-7-phosphaadamantane complexes of rhodium and ruthenium has been found to be catalytically active for the conversion of aldehydes to alcohols [13, 14] .

In the title compound the Ag atom is in a four-coordinate environment and adopts a distorted tetrahedral geometry, with the Ag and Cl atoms on special positions. As the complex crystallizes with high symmetry the Ag—P bond lengths are identical: 2.4676(4) Å. The P—Ag—P angles of the title compound are either 108.67(1)° or 111.08(1)° and the effective cone angle [15] is 108.53(1)°. The crystal structure is stabilized by an array of weak C—H⋅⋅⋅Cl and strong O—H⋅⋅⋅N hydrogen bonds. The title structure is structurally closely related to a Au(I) complex [16].

Acknowledgement

Financial assistance from the University of the Free State is gratefully acknowledged. This work is based on the research supported in part by the National Research Foundation of South Africa, Unique Grants No. 93957 and 99139.

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Received: 2017-3-2
Accepted: 2017-7-27
Published Online: 2017-8-11
Published in Print: 2017-9-26

©2017 Runé Oosthuizen et al., published by De Gruyter, Berlin/Boston

This work is licensed under the Creative Commons Attribution-NonCommercial-NoDerivatives 4.0 License.

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