Li-Na Cui

catena-Poly[silver(I)-bis­[μ-bis­(diphenyl­phosphino)methane-κ2P:P′]-μ-thio­cyanato-κ2S:S-silver(I)-μ-thio­cyanato-κ2S:N]

The title compound, [Ag(NCS)(C25H22P2)]n, contains two Ag+ ions, two thiocyanate ions and two bis(diphenylphosphino)methane (dppm) ligands in the asymmetric unit. One of the thiocyanate ions bridges the two Ag+ ions in a μ2-mode from its S atom and the two dppm ligands bridge the silver ions in a μ1,μ1 mode. The remaining SCN− ion bridges the binuclear units via its N and S atoms, generating a one-dimensional polymer propagating in [01]: the resulting AgP2SN and AgP2S2 coordination geometries could be described as distorted tetrahedral.

(Methanol-κO)(perchlorato-κO)bis-(triphenyl-phosphine-κP)silver(I).

In the title complex, [Ag(ClO4)(CH3OH)(C18H15P)2], the angles around the central Ag+ ion indicate that it is in a distorted tetrahedral coordination. The coordination sphere of silver is formed by two P atoms of two triphenylphosphine ligands, one O atom of a perchlorate anion and one O atom of a methanol molecule. The crystal structure is stablized by a bifurcated intermolecular O—H⋯O hydrogen bond, involving the O—H donor from methanol and two acceptor O atoms from the perchlorate anion, so forming a zigzag chain propagating in [010].

(Perchlorato-κO)tris­(triphenyl­phosphine-κP)silver(I)

In the title complex, [Ag(C18H15P)3(ClO4)], the silver coordination environment is dominated by the distorted P3AgO tetrahedron in which Ag—O = 2.608 (12) Å and the Ag—P bond lengths are 2.5663 (17), 2.5076(16) and 2.5450 (17) Å. The perchlorate O-atoms are disordered over two positions in a 0.584 (14):0.416 (14) ratio.

Bis(2,2′-bi-1H-imidazole-κ2 N 3,N 3′)bis­(dimethyl sulfoxide-κO)copper(II) bis­(tetra­fluoridoborate)

In the title copper(II) salt, [Cu(C6H6N4)2(C2H6OS)2](BF4)2, the Jahn–Teller distorted octahedral coordination sphere of copper is formed from four 2,2′-bi-1H-imidazole N atoms and two dimethyl sulfoxide O atoms. The Cu atom lies on a center of inversion. N—H⋯O and N—H⋯F hydrogen bonds give rise to a one-dimensional structure. The BF4 − anion is disordered over two sites in a 0.671 (10):0.329 (10) ratio.

Tris(3-amino-5,6-dimethyl-1,2,4-triazine-κN)silver(I) trifluromethane-sulfonate-3-amino-5,6-dimethyl-1,2,4-triazine (1/1).

The asymmetric unit of the title compound, [Ag(C5H8N4)3](CF3O3S)·C5H8N4, contains two cations, two anions and two uncoordinated 3-amino-5,6-dimethyl-1,2,4-triazine (admt) ligands. It was prepared from the reaction of silver trifluoromethanesulfonate and admt in a 2:3 molar ratio. Both silver(I) ions are bonded to three admt molecules via their 2-position triazine N atoms in almost regular trigonal–planar geometries. Three intramolecular N—H⋯N hydrogen bonds between adjacent admt molecules in each cation help to maintain their overall near planarities (r.m.s. deviations for the 28 non-H atoms = 0.139 and 0.153 Å). In the crystal, numerous N—H⋯N, N—H⋯O, C—H⋯O, C—H⋯N and C—H⋯F hydrogen-bonding interactions link the components into a three-dimensional network.

Tetra-kis(triphenyl-phosphane-κP)silver(I) trifluoro-methane-sulfonate dichloro-methane monosolvate.

In the title compound, [Ag(C18H15P)4]CF3O3S·CH2Cl2, the Ag atom is coordinated by four P atoms from four PPh3 ligands. The P—Ag—P angles are in the range 108.02 (6)–110.15 (6)°, which confirms the distorted tetrahedral environment around the Ag atom.

Crystal structure of bis(triphenylphospine-kP)-dichloropalladium( II) —acetonitrile (1:1), [PdCl2(C18H15P)2] · CH3CN

C38H33Cl2NP2Pd, monoclinic, C12/c1 (no. 15), a = 12.056(1) Å, b = 14.393(1) Å, c = 20.002(2) Å, * = 92.372(1)°, V = 3467.8 Å, Z = 4, Rgt(F) = 0.070, wRref(F ) = 0.178, T = 298 K.

Poly[bis­[μ-1,3-bis­(diphenyl­phosphan­yl)propane-κ2P:P′]-di-μ-thio­cyanato-κ2S:N;κ2N:S-disilver(I)]

In the title coordination polymer, [Ag2(NCS)2(C27H26P2)2]n, two centrosymmetrically related Ag+ cations are linked by two thiocyanate anions into binuclear eight-membered macrocycles. The Ag⋯Ag separation within the macrocycle is 5.4400 (6) Å. The distorted tetrahedral coordination about each metal atom is completed by the P atoms of two bridging 1,3-bis(diphenylphosphanyl)propane ligands, forming polymeric ribbons parallel to the a axis.

Crystal structure of bis(triphenylphosphine)(acetato-O,O′)silver(I) — hydrate —methanol (2:1:1), [Ag(PPh3)2(CH3COO)]2 · H2O · CH3OH

C77H72Ag2O6P4, monoclinic, C12/c1 (no. 15), a = 44.268(2) Å, b = 13.2848(5) Å, c = 24.9524(9) Å, * = 105.449(2)°, V = 14144.1 Å, Z = 8, Rgt(F) = 0.067, wRref(F) = 0.143, T = 296 K. Source of material A mixture of AgCH3COO (silver acetate), PPh3 (triphenylphosphine) and C4H5N3 (2-AMP = 2-aminopyrimidine) in molar ratio of 1:1:2 in CH2Cl2/CH3OH (10 ml, v/v = 1/1) was stirred for 2 hours at room temperature, then filtered. Subsequent slow evaporation of the filtrate resulted in the formation of colorless crystals of the title complex. Crystals suitable for single crystal X-ray diffraction were selected directly from the sample as prepared. Discussion For extending study on systematic structural chemistry of silver complexes of ligands containing P and N atoms, such as [Ag(.X)(2-Apy)(PPh3)]2 (X = Cl, Br) [1], [Ag2(.-dppm)2(.-SO4)(2AMP)2] · CH3OH [2], [Ag2Cl2(PPh3)2(2-AMP)]∞ [3] [Ag2Br2(PPh3)2(2-AMP)]∞ [4], we synthesized a new complex with the formula [Ag(PPh3)2(CH3COO)]2 · H2O · CH3OH in the presence of 2-aminopyridine by the similar reaction as the two similar complexes [Ag(PPh3)2(CH3OH)(ClO4)] and [Ag(PPh3)3(ClO4)] [5]. The title complex consists of two [Ag(PPh3)2(CH3COO)] units, a water molecule and a methanol molecule. Both the two silver atoms are four-coordinated with a AgP2O2 environment, where two phosphorus atoms are from PPh3 with d(Ag—P) ranging from 2.398(2) Å to 2.453(2) Å, two oxygen atoms are from CH3COO with the d(Ag—O) in the range of 2.395(5) Å 2.450(5) Å. The bond angles ∠P–Ag–O are in the range of 102.32(1) 121.2(2)°, the bond angles ∠P–Ag–P are in the range of 128.13° 128.27(6)°, the bond angles ∠O–Ag–O are 52.8(2)° and 53.6(2)°, which comfirm the distorted tetrahedral environment around the silver atom. Two [Ag(PPh3)2(CH3COO)] units are linked via hydrogen bond O6–H6A···O1 (with d(O6···O1) = 2.873 Å and ∠O6–H6A–O1 of 173.27°) and hydrogen bond O6–H6B···O3 (with d(O6···O3) = 2.841 Å and ∠O6–H6–O1 = 171.28°). The compound is further stablized by hydrogen bond O5–H5A···O2 formed between O–H donor of methanol and O atom of acetate anion with d(O5···O2) = 2.795 Å and ∠O5–H5A–O2 = 170.69°. The similar complex AgCH3COO · PPh3 · dmp · MeOH [6] has d(Ag—P) = 2.3792(3) Å, and d(Ag—O) = 2.3993(9) Å and 2.875(1) Å, but the silver atom is five-coordinated. Z. Kristallogr. NCS 225 (2010) 645-648 / DOI 10.1524/ncrs.2010.0282 645