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1.
Synthesis and Crystal Structure of Metal(I) Hydrogen Sulfates – Ag(H3O)(HSO4)2, Ag2(HSO4)2(H2SO4), AgHSO4, and Hg2(HSO4)2 Hydrogen sulfates Ag(H3O)(HSO4)2, Ag2(HSO4)2 · (H2SO4), and AgHSO4 have been synthesized from Ag2SO4 and sulfuric acid. Hg2(HSO4)2 was obtained from metallic mercury and 96% sulfuric acid as starting materials. The compounds were characterized by X‐ray single crystal structure determination. Ag(H3O)(HSO4)2 belongs to the structure type of Na(H3O)(HSO4). The silver atom is coordinated by 6 + 2 oxygen atoms. In the structure, there are dimers and chains of hydrogen bonded HSO4 tetrahedra. Dimers and chains are connected by the H3O+ ion to form a three dimensional hydrogen network. Ag2(HSO4)2(H2SO4) crystallizes isotypic to Na2(HSO4)2(H2SO4). The coordination number of silver is 6 + 1. The structure of Ag2(HSO4)2(H2SO4) is characterized by hydrogen bonded trimers of HSO4 tetrahedra, which are further connected to chains. For the recently published structure of AgHSO4 the hydrogen bonding system was discussed. There are tetrameres and chains, connected by bifurcated hydrogen bonds. The structure of Hg2(HSO4)2 contains Hg22+ cations with Hg–Hg distance of 2.509 Å. Every mercury atom is coordinated by one oxygen atom at shorter distance (2.18 Å) and three ones at longer distances (2.57 to 3.08 Å). The HSO4 tetrahedra form zigzag chains by hydrogen bonds.  相似文献   

2.
New platinum-mercury clusters, Pt4(HgX)2(μ-CO)4(PR3)4 (X=Cl, Br, I, CF3, or CCl3; R=Ph or Et), were synthesized. The molecular and crystal structure of the Pt4(HgBr)2(μ-CO)4(PPh3)4 cluster was established by X-ray structural analysis.  相似文献   

3.
New Phosphido-bridged Multinuclear Complexes of Ag and Zn. The Crystal Structures of [Ag3(PPh2)3(PnBu2tBu)3], [Ag4(PPh2)4(PR3)4] (PR3 = PMenPr2, PnPr3), [Ag4(PPh2)4(PEt3)4]n, [Zn4(PPh2)4Cl4(PRR′2)2] (PRR′2 = PMenPr2, PnBu3, PEt2Ph), [Zn4(PhPSiMe3)4Cl4(C4H8O)2] and [Zn4(PtBu2)4Cl4] AgCl reacts with Ph2PSiMe3 in the presence of tertiary Phosphines (PnBu2tBu, PMenPr2, PnPr3 and PEt3) to form the multinuclear complexes [Ag3(PPh2)3(PnBu2tBu)3] 1 , [Ag4(PPh2)4(PR3)4] (PR3 = PMenPr2 2 , PnPr3 3 ) and [Ag4(PPh2)4(PEt3)4]n 4 . In analogy to that ZnCl2 reacts with Ph2PSiMe3 and PRR′2 to form the multinuclear complexes [Zn4(PPh2)4Cl4(PRR′2)2] (PRR′2 = PMenPr2 5 , PnBu3 6 , PEt2Ph 7 ). Further it was possible to obtain the compounds [Zn4(PhPSiMe3)4Cl4(C4H8O)2] 8 and [Zn4(PtBu2)4Cl4] 9 by reaction of ZnCl2 with PhP(SiMe3)2 and tBu2PSiMe3, respectively. The structures were characterized by X-ray single crystal structure analysis. Crystallographic data see “Inhaltsübersicht”.  相似文献   

4.
Red single crystals of Gd2[Pt2(SO4)4(HSO4)2](HSO4)2 (triclinic, , Z = 1, a = 844.02(9), b = 908.50(9), c = 939.49(8) pm, α = 107.73(1)°, β = 112.10(1)°, γ = 103.53(1)°) were obtained by the reaction of [Gd(NO3)(H2O)7][PtCl6]·4H2O with sulfuric acid at 320 °C in a sealed glass ampoule. In the crystal structure, Pt2 dumbbells are coordinated by four chelating sulfate groups and two monodentate hydrogensulfate ions. Two further HSO4? ions are not bonded to the Pt2 dumbbell. The Gd3+ ions are eightfold coordinated by oxygen atoms. The IR data of Gd2[Pt2(SO4)4(HSO4)2](HSO4)2 are typical for these type of compounds. The thermal decomposition of the compound leads to elemental platinum and Gd2O3.  相似文献   

5.
(Hg2)Hg(OH)2(ClO4)2: The First Mixed Valent Mercury Perchlorate Colorless single crystals of (Hg2)Hg(OH)2(ClO4)2 (C2/c, Z = 4, a = 1847.7(5), b = 490.8(1), c = 1086.2(3) pm, β = 93.80(2)°, Rall = 0.0610) were obtained as a side product during the dehydration of Hg2(ClO4)2 · 2H2O. The crystal structure consists of infinite zig‐zag chains {1[(Hg2)1/2(OH)Hg1/2]+}2 which are separated by the ClO4 ions.  相似文献   

6.
Red single crystals of Pt2(HSO4)2(SO4)2 were obtained by the reaction of elemental platinum with conc. sulfuric acid at 350 °C in sealed glass ampoules. The crystal structure (monoclinic, P21/c, Z = 2, a = 868.6(2), b = 826.2(1), c = 921.8(2) pm, β=116.32(1)°, Rall = 0.0348) shows dumbbell shaped Pt26+ cations which are coordinated by four SO42— and two HSO4 ions. Each of the sulfate ions is attached to another Pt26+ ion yielding layers according to equation/tex2gif-stack-1.gif[Pt2(SO4)4/2(HSO4)2/1]. The layers are connected by hydrogen bonds with the OH group of the hydrogensulfate ion as donor and the non‐bonding oxygen atom of the sulfate ion as acceptor.  相似文献   

7.
Synthesis and Crystal Structure of K2(HSO4)(H2PO4), K4(HSO4)3(H2PO4), and Na(HSO4)(H3PO4) Mixed hydrogen sulfate phosphates K2(HSO4)(H2PO4), K4(HSO4)3(H2PO4) and Na(HSO4)(H3PO4) were synthesized and characterized by X‐ray single crystal analysis. In case of K2(HSO4)(H2PO4) neutron powder diffraction was used additionally. For this compound an unknown supercell was found. According to X‐ray crystal structure analysis, the compounds have the following crystal data: K2(HSO4)(H2PO4) (T = 298 K), monoclinic, space group P 21/c, a = 11.150(4) Å, b = 7.371(2) Å, c = 9.436(3) Å, β = 92.29(3)°, V = 774.9(4) Å3, Z = 4, R1 = 0.039; K4(HSO4)3(H2PO4) (T = 298 K), triclinic, space group P 1, a = 7.217(8) Å, b = 7.521(9) Å, c = 7.574(8) Å, α = 71.52(1)°, β = 88.28(1)°, γ = 86.20(1)°, V = 389.1(8)Å3, Z = 1, R1 = 0.031; Na(HSO4)(H3PO4) (T = 298 K), monoclinic, space group P 21, a = 5.449(1) Å, b = 6.832(1) Å, c = 8.718(2) Å, β = 95.88(3)°, V = 322.8(1) Å3, Z = 2, R1 = 0,032. The metal atoms are coordinated by 8 or 9 oxygen atoms. The structure of K2(HSO4)(H2PO4) is characterized by hydrogen bonded chains of mixed HnS/PO4 tetrahedra. In the structure of K4(HSO4)3(H2PO4), there are dimers of HnS/PO4 tetrahedra, which are further connected to chains. Additional HSO4 tetrahedra are linked to these chains. In the structure of Na(HSO4)(H3PO4) the HSO4 tetrahedra and H3PO4 molecules form layers by hydrogen bonds.  相似文献   

8.
Bis(disulfido)bridged NbIV cluster oxalate complexes [Nb2(S2)2(C2O4)4]4– were prepared by ligand substitution reaction from the aqua ion [Nb2(μ‐S2)2(H2O)8]4+ and isolated as K4[Nb2(S2)2(C2O4)4] · 6 H2O ( 1 ), (NH4)6[Nb2(S2)2(C2O4)4](C2O4) ( 2 ) and Cs4[Nb2(S2)2(C2O4)4] · 4 H2O ( 3 ). The crystal structures of 1 and 2 were determined. The crystals of 1 belong to the space group P1, a = 720.94(7) pm, b = 983.64(10) pm, c = 1071.45(10) pm, α = 109.812(1)°, β = 91.586(2)°, γ = 105.257(2)°. The crystals of 2 are monoclinic, space group C2/c, a = 1567.9(2) pm, b = 1906.6(3) pm, c = 3000.9(4) pm, β = 95.502(2)°. The packing in 2 shows alternating layers of cluster anions and of ammonium/uncoordinated oxalates perpendicular to the [1 0 1] direction. Vibration spectra, electrochemistry and thermogravimetric properties of the complexes are also discussed.  相似文献   

9.
The crystal structures of Na2Mg3(OH)2(SO4)3 · 4H2O and K2Mg3(OH)2(SO4)3 · 2H2O, were determined from conventional laboratory X‐ray powder diffraction data. Synthesis and crystal growth were made by mixing alkali metal sulfate, magnesium sulfate hydrate, and magnesium oxide with small amounts of water followed by heating at 150 °C. The compounds crystallize in space group Cmc21 (No. 36) with lattice parameters of a = 19.7351(3), b = 7.2228(2), c = 10.0285(2) Å for the sodium and a = 17.9427(2), b = 7.5184(1), c = 9.7945(1) Å for the potassium sample. The crystal structure consists of a linked MgO6–SO4 layered network, where the space between the layers is filled with either potassium (K+) or Na+‐2H2O units. The potassium‐bearing structure is isostructural to K2Co3(OH)2(SO4)3 · 2(H2O). The sodium compound has a similar crystal structure, where the bigger potassium ion is replaced by sodium ions and twice as many water molecules. Geometry optimization of the hydrogen positions were made with an empirical energy code.  相似文献   

10.
Syntheses and Crystal Structures of [Cu4(As4Ph4)2(PRR′2)4], [Cu14(AsPh)6(SCN)2(PEt2Ph)8], [Cu14(AsPh)6Cl2(PRR′2)8], [Cu12(AsPh)6(PPh3)6], [Cu10(AsPh)4Cl2(PMe3)8], [Cu12(AsSiMe3)6(PRR′2)6], and [Cu8(AsSiMe3)4(PtBu3)4] (R, R′ = Organic Groups) Through the reaction of CuSCN with AsPh(SiMe3)2 in the presence of tertiary phosphines the compounds [Cu4(As4Ph4)2(PRR′2)4] ( 1 – 3 ) ( 1 : R = R′ = nPr, 2 : R = R′ = Et; 3 : R = Me, R′ = nPr) and [Cu14(AsPh)6(SCN)2(PEt2Ph)8] ( 4 ) can be synthesised. Using CuCl instead of CuSCN results to the cluster complexes [Cu14(AsPh)6Cl2(PRR′2)8] ( 5–6 ) ( 5 : R = R′ = Et; 6 : R = Me, R′ = nPr), [Cu12(AsPh)6(PPh3)6] ( 7 ) and [Cu10(AsPh)4Cl2(PMe3)8] ( 8 ). Through reactions of CuOAc with As(SiMe3)3 in the presence of tertiary phosphines the compounds [Cu12(AsSiMe3)6(PRR′2)6] ( 9 – 11 ) ( 9 : R = R′ = Et; 10 : R = Ph, R′ = Et; 11 : R = Et, R′ = Ph) and [Cu8(AsSiMe3)4(PtBu3)4] ( 12 ) can be obtained. In each case the products were characterised by single‐crystal‐X‐ray‐structure‐analyses. As the main structure element 1 – 3 each have two As4Ph42–‐chains as ligands. In contrast 4 – 12 contain discrete AsR2–ligands.  相似文献   

11.
The compound (NH4)2[Re2(HPO4)4 · 2H2O] has been synthesized and characterized by electronic and vibrational spectroscopy. The molecular structure has been determined by X-ray diffraction (MoK α radiation, λ = 0.71073 Å). The (NH4)2[Re2(HPO4)4 · 2H2O] coordination units form centrosymmetrical binuclear ordering with each metal atom being coordinated in a distorted octahedron incorporating one rhenium atom, one oxygen atom of the water molecule, and four phosphate oxygen atoms in the equatorial plane. The rhenium-rhenium bond length (2.2207 Å) corresponds to a quadruple bond between the atoms. The [Re2(HPO4)4 · 2H2O]2- complex anions in the crystal are associated through strong hydrogen bonds formed by the phosphate O-H···O groups. The stability of dirhenium(III) tetra-μ-phosphates in aqueous solutions is considered.  相似文献   

12.
On a New Complex of Antimony Oxide Fluoride and Oxalate. Crystal Structure of (NH4)4H2(C2O4)3(SbOF) 2 · H2O The crystal structure of (NH4)4H2(C2O4)3(SbOF) 2 · H2O has been fixed by X-ray diffraction on single crystal (R = 0.025 for 2124 planes). The antimony atom is complexed by the oxalate anions which are bidendate chelates. Antimony coordination is seven (five oxygen atoms, one fluorine atom, and the lone pair E). Antimony environment is a pentagonal bipyramid, one of the axial positions is occupied by the lone pair, the other one by the fluorine atom.  相似文献   

13.
New Phosphido-bridged Multinuclear Complexes of Ag, Cd and Zn. The Crystal Structures of [Ag4(PPh2)4(PMe3)4], [Ag6(PPh2)6(PtBu3)2] and [M4Cl4(PPh2)4(PnPr3)2] (M = Zn, Cd) AgCl reacts with Ph2PSiMe3 in the presence of a tertiary Phosphine PMe3 or PtBu3 to form the multinuclear complexes [Ag4(PPh2)4(PMe3)4] ( 1 ) and [Ag6(PPh2)6(PtBu3)2] ( 2 ). In analogy to that MCl2 reacts with Ph2PSiMe3 in the presence of PnPr3 to form the two multinuclear complexes [M4Cl4(PPh2)4(PnPr3)2] (M = Zn ( 3 ), Cd ( 4 )). The structures were characterized by X-ray single crystal structure analysis ( 1 : space group Pna21 (Nr. 33), Z = 4, a = 1 313.8(11) pm, b = 1 511.1(6) pm, c = 4 126.0(18) pm, 2 : space group P1 (Nr. 2), Z = 2, a = 1 559.0(4) pm, b = 1 885.9(7) pm, c = 2 112.4(8) pm, α = 104.93(3)°, β = 94.48(3)°, γ = 104.41(3)°; 3 : space group C2/c (Nr. 15), Z = 4, a = 2 228.6(6) pm, b = 1 847.6(6) pm, c = 1 827.3(6) pm, β = 110.86(2); 4 : space group C2/c (Nr. 15), Z = 4, a = 1 894.2(9) pm, b = 1 867.9(7) pm, c = 2 264.8(6) pm, β = 111.77(3)°). 3 and 4 may be considered as intermediates on the route towards polymeric [M(PPh2)2]n (M = Zn, Cd).  相似文献   

14.
AgCo3PO4(HPO4)2     
The structure of the hydro­thermally synthesized compound AgCo3PO4(HPO4)2, silver tricobalt phosphate bis­(hydrogen phosphate), consists of edge‐sharing CoO6 chains linked together by the phosphate groups and hydrogen bonds. The three‐dimensional framework delimits two types of tunnels which accommodate Ag+ cations and OH groups. The title compound is isostructural with the compounds AM3H2(XO4)3 (A = Na or Ag, M = Co or Mn, and X = P or As) of the alluaudite structure type.  相似文献   

15.
Reaction of a mixture of neodymium carbonate, HCl, oxamic acid and glutaric acid under hydrothermal conditions gives rise to a new mixed carboxylate of neodymium, [Nd4(H2O)2(OOC(CH2)3COO)4(C2O4)2], I. The structure, determined using single crystal X-ray diffraction, comprises a helical column formed by the grafting of the oxalate unit on to helical NdO9 chains, cross-linked by the glutarate anions. It is noteworthy that the pitch of the helix is equivalent to the length of the oxalate unit. Furthermore, I shows about 1.1 times the SHG activity of urea.  相似文献   

16.
The Tl2MoO4-Nd2(MoO4)3-Hf(MoO4)2 system was studied in the subsolidus region using X-ray powder diffraction. New triple molybdates were found to exist in this system: Tl5NdHf(MoO4)6 (5: 1: 2), TlNdHf0.5(MoO4)3 (1: 1: 1), and Tl2NdHf2(MoO4)6.5 (2: 1: 4). The first TlNd(MoO4)2 single crystals were grown from melt solutions with spontaneous nucleation. Their crystal structure was refined from X-ray diffraction data (Bruker X8 Apex automated diffractometer, MoK α radiation, 386 F(hkl), R = 0.0136). The tetragonal unit cell parameters are as follows: a = 6.3000(2) Å, c = 9.5188(5) Å, V = 377.80(3) Å3, Z = 2, ρcalcd = 5.876 g/cm3, space group P4/nnc. The structure is a framework built of NdO8 and TlO8 tetragonal antiprisms linked via shared lateral edges and alternating in the checkerboard order. Layers share oxygen vertices with MoO4 interlayer tetrahedra and are linked into the framework.  相似文献   

17.
Two novel isopropylamine‐templated uranyl chromates, [(CH3)2CHNH3]3[(UO2)3(CrO4)2O(OH)3] ( 1 ) and [(CH3)2CHNH3]2[(UO2)2(CrO4)3(H2O)] ( 2 ) were prepared by hydrothermal method at 100 °C. The compounds were characterized by electron microprobe analysis and X‐ray diffraction crystal structure analysis [ 1 : trigonal, P31m, a = 9.646(4), c = 8.469(4) Å, V = 682.4(5) Å3; 2 : monoclinic, P21/c, a = 11.309(3), b = 11.465(3), c = 17.055(5) Å, β = 99.150(6)°, V = 2183.2(11) Å3]. The structure of 1 is based upon trimers of uranyl bipyramids interlinked by CrO4 tetrahedra to form [(UO2)3(CrO4)2O(OH)3]3– layers, whereas, in the structure of 2 , UO7 and UO6(H2O) pentagonal bipyramids are linked through CrO4 tetrahedra into the [(UO2)2(CrO4)3(H2O)]2– layers. The structures show many similarities to related uranyl selenate compounds, thus providing additional data on similarities and differences between uranyl sulfates, chromates, selenates, and molybdates.  相似文献   

18.
Reaction of NiCl2 with PhP(SiMe3)2, The Crystal Structure of [Ni12Cl2(PPh)2(P2Ph2)4(PHPh)8] [Ni12Cl2(PPh)2(P2Ph2)4(PHPh)8] ( 1 ) has been prepared by the reaction of NiCl2 with PhP(SiMe3)2. The structure has been characterized by X-ray crystal structure analysis. 1 contains a Ni12-cluster with m?4-PPh- and m?6-P2Ph2- as bridging ligands. The terminal PHPh- and Cl-ligands are bound to Ni-atoms. The Ni12-cluster can be described as an Ni8-cube, in which four edges are bridged by Ni-atoms.  相似文献   

19.
Green single crystals of trans‐tetraamminedibromidochromium(III) trans‐diamminetetrabromidochromate(III), [CrBr2(NH3)4][CrBr4(NH3)2], are found to contain two symmetry‐independent sixfold coordinated CrIII cations on centres of inversion. The structure is composed of octahedral trans‐[CrBr2(NH3)4]+ cations and octahedral trans‐[CrBr4(NH3)2] anions, and adopts a distorted CsCl‐type lattice. The cations and anions are linked by N—H...Br interactions. This is the first example in which both ions are mixed ammine–bromide CrIII complexes.  相似文献   

20.
The glass formation region boundaries were found in the systems Al2(SO4)3-MSO4-H2O, where M = Cd2+, Zn2+, and Mg2+, and Al2(SO4)3-Fe2(SO4)3-H2O. The causes of the differences in glass-forming ability between the studied systems were analyzed. The structures and properties of glassy Al2(SO4)3 · 11H2O and Fe2(SO4)3 · 11H2O were compared.  相似文献   

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