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1.
By means of X-ray diffraction the chain structure of [Cu(l-Arg)2]Hg2Cl6 (monoclinic, a = 10.2348(9) Å, b = 9.1386(7) Å, c = 14.8521(14) Å, β = 97.455(11)°, space group P21) is established. The chains are formed by square-planar [Cu(l-Arg)2]2+ cations of the type trans-[Cu(N)2(O)2] (l-Arg is the zwitter-ion of arginine; Cu-N 1.992 Å and 1.938(6) Å, Cu-O 1.953 Å and 1.967(4) Å) that are bonded to two adjacent binuclear [Cl2Hg(μ-Cl)2HgCl2]2? ions through its clorine atoms Cl (Hg-Cl bonds are within 2.34–2.78 Å). With these two additional Cu…Cl contacts Cu adopts the geometry of an elongated octahedron with two apical Cl (Cu-Cl 2.961 Å and 3.064(3) Å). 相似文献
2.
Molybdenum(II) Halide Clusters with two Alcoholate Ligands: Syntheses and Crystal Structures of (C18H36N2O6Na)2[Mo6Cl12(OCH3)2] and (C18H36N2O6Na)2[Mo6Cl12(OC15H11)2] · 2C4H6O3 . Reaction of Mo6Cl12 with two equivalents of sodium methoxide in the presence of 2,2,2-crypt yields (C18H36N2O6Na)2[Mo6Cl12(OCH3)2] ( 1 ), which can be converted to (C18H36N2O6Na)2[Mo6Cl12(OC15H11)2] · 2C4H6O3 ( 2 ) by metathesis with 9-Anthracenemethanole in propylene carbonate. As confirmed by X-ray single crystal structure determination ( 1 : C2/m, a=25.513(8) Å, b=13.001(3) Å, c=10.128(3) Å, β=100.204(12)°; : C2/c, a=15.580(5) Å, b=22.337(5) Å, c=27.143(8) Å, β=98.756(10)°) the compounds contain anionic cluster units [Mo6ClCl(ORa)2]2? with two alcoholate ligands in terminal trans positions ( 1 : d(Mo—Mo) 2.597(2) Å to 2.610(2) Å, d(Mo—Cli) 2.471(3) Å to 2.493(4) Å, d(Mo—Cla) 2.417(8) Å and 2.427(8) Å, d(Mo—O) 2.006(13) Å; 2 : d(Mo—Mo) 2.599(3) Å to 2.628(3), d(Mo—Cli) 2.468(8) Å to 2.506(7) Å, d(Mo—Cla) 2.444(8) Å and 2.445(7) Å, d(Mo—O) 2.012(19) Å). 相似文献
3.
Ag2Pb8O7Cl4, a New Member of Lead(II) Oxyhalides with Silver Ag2Pb8O7Cl4 is one among other products of the thermal decomposition of AgPb4O4Cl. Ag2Pb8O7Cl4 can be prepared directly by heating the binary components within a temperature range from 590°C to 620°C. The crystal structure was solved by single crystal X-ray methods. The compound crystallizes monoclinic with a = 12.411(4) Å, b = 17.99(3) Å, c = 14.785(4) Å, β = 147.01(2)°, Z = 4 with the space group P21/c. Ag2Pb8O7Cl4 shows remarkable structural features, e.g. silver tetrahedrally surrounded by chlorine. 相似文献
4.
Molybdenum(II) Halide Clusters with six Alcoholate Ligands: (C18H36N2O6Na)2[Mo6Cl8(OCH3)6] · 6CH3OH and (C18H36N2O6Na)2[Mo6Cl8(OC6H5)6] . The reaction of Na2[Mo6Cl8(OCH3)6] and 2,2,2-crypt yields (C18H36N2O6Na)2[Mo6Cl8(OCH3)6] · 6 CH3OH ( 1 ), which is converted to (C18H36N2O6Na)2[Mo6Cl8(OC6H5)6] ( 2 ) by metathesis with phenol. According to single crystal structure determinations ( 1 : P3 1c, a=14.613(3) Å, c=21.036(8) Å; 2 : P3 1c, a=15.624(1) Å, c=19.671(2) Å) the compounds contain anionic clusters [Mo6Cl8i(ORa)6]2? ( 1 : d(Mo—Mo) 2.608(1) Å to 2.611(1) Å, d(Mo—Cl) 2.489(1) Å to 2.503(1) Å, d(Mo—O) 2.046(4) Å; 2 : d(Mo—Mo) 2.602(3) Å to 2.608(3) Å, d(Mo—Cl) 2.471(5) Å to 2.4992(5) Å, d(Mo—O) 2.091(14) Å). Electronic interactions of the halide cluster and the phenolate ligands in [Mo6Cl8(OC6H5)6]2? is investigated by means of UV/VIS spectroscopy and EHMO calculations. 相似文献
5.
Structure‐Behaviour‐Relation of Cu5Pb6O3Cl11, a Good Solid State Ionic Conductor for Cu+‐Ions A new compound within the group of coin metal lead(II) oxide halides is found and characterized by X‐ray single crystal structure determination in a temperature range from 120 K to 400 K. Cu5Pb6O3Cl11 shows a new crystal type structure with a = 21.098(4) Å, b = 10.233(2) Å, c = 12.224(2) Å, β = 124.08(3)°, Z = 4 and space group C 2/c (No. 15) at 120 K. There are found isolated oxidic chains built of OPb4 tetrahedra beside columnar areas consisting of CuCl. In this halidic partial structure are a lot of empty and partially occupied Cl4‐tetrahedra. This structural characteristic seems to be source of a very good conductivity of copper ions, like in microscopic and nanoscaled composites of Al2O3 and AgI. 相似文献
6.
Caesiumchloropalladate(II)‐hydrates – Two New Compounds with Condensed [Pd2Cl6] Groups We were able to synthesize two caesiumchloropalladate(II)‐hydrates in the CsCl/PdCl2/H2O system by hydrothermal methods. Both compounds show combination of monomeric and dimeric Pd–Cl groups. We characterized the crystal structures by single‐crystal X‐ray diffraction. Cs6Pd5Cl16 · 2 H2O ( I ) crystallizes triclinic in space group type P1 (Nr. 2) with a = 8.972(1) Å, b = 11.359(1) Å, c = 18.168(1) Å, α = 83.61(1)°, β = 76.98(1)°, γ = 76.39(1)° and Z = 2, Cs12Pd9Cl30 · 2 H2O ( II ) monoclinic, space group type C2/m (No. 12) with a = 19.952(1) Å, b = 14.428(1) Å, c = 14.411(1) Å, β = 125.29(1)°, and Z = 2. 相似文献
7.
Crystals of [Cu(Eddp)·(HgCl2)3]n (monoclinic, a = 9.7547(7) Å, b = 18.3716(12) Å, c = 11.7811(9) Å, β = 94.828(9)°, Z = 4, space group P21/n) are made of infinite sheets involving dimeric complexes [Cu2(Eddp)2] interacting with quasi-molecules of HgCl2 (Hg-Cl 2.29-2.36 Å). In the dimers, copper atoms are squarely surrounded by two N atoms and two O atoms of the ethylendiamine-N,N′-di(3-propionate) anion, and atom from a neighboring Eddp ion in the apical position; the second apical position is occupied by a Cl atom of one of HgCl2 molecules. Weak Hg-Cl interactions (2.98-3.07 Å) join the molecules of HgCl2 in almost planar centrosymmetrical Hg6Cl12 hexamers, and further (Hg-Cl 3.168(3) Å, 3.250(2) Å) in infinite chains of the hexamers. Finally, the dimeric copper complexes are linked to six Hg atoms of four adjacent hexamers by virtue of their oxygen atoms (Hg-O 2.322(8), 2.609(6) Å, 2.730(5) Å). 相似文献
8.
Inhaltsübersicht. Die erstmals dargestellte Verbindung HgPb2O(OH)Br3 kristallisiert orthorhombisch in der Raumgruppe Aba2 (Nr. 41) mit den Gitterkonstanten a = 14,652(3) Å, b = 14,6491(8) Å, c = 7,782(2) Å und Z = 8. Die Bestimmung der Kristallstruktur mit Einkristallmethoden zeigte “isolierte”, verzerrt würfelförmige Baugruppen der Zusammensetzung [Hg2Pb4O2(OH)2]. Diese Einheiten werden von Bromidionen umhüllt. HgPb2O(OH)Br3 stellt damit hinsichtlich des strukturellen Aufbaus ein Bindeglied zwischen den Verbindungen [Pb4(OH)4](ClO4)4 · 2H2O [1] und Pb9O4Br10 [2] dar. Preparation and Crystal Structure of HgPb2O(OH)Br3 The new compound, HgPb2O(OH)Br3 was prepared and investigated by X-ray crystal structure analysis. Crystals of orthorhombic symmetry show space group Aba2 (No. 41) with lattice parameters a = 14.652(3) Å, b = 14.6491(8) Å, c = 7.782(2) Å, and Z = 8. Remarcable structural units with heterocubane skeleton were found. The [Hg2Pb4O2(OH)2] group forms a new member of the structural class between [Pb4(OH)4] and [Pb8O4] units with the relating compounds [Pb4(OH)4)](ClO4)4 · 2 H2O [1] und Pb9O4Br10 [2]. 相似文献
9.
Barbara Schüpp Liane Schrder Helga Schulte Carsten Bhtz Norbert Mattern Hans‐Lothar Keller 《无机化学与普通化学杂志》2002,628(7):1708-1714
Hochtemperatur‐Cs2[PdCl4] — New Results on a “wellknown” Compound Two modifications of Cs2[PdCl4] have been characterized by X‐ray powder and single crystal diffraction, respectively. The crystal structures are described and the group‐subgroup‐relations between these structures are discussed. In addition to the tetragonal (P4/mmm (No. 123), a = 7.4158(8) Å, c = 4.6792(6) Å) and the orthorhombic (Cmcm (No. 63), a = 10.529(1) Å, b = 10.310(1) Å, c = 9.460(1) Å) modification DSC investigations and high‐temperature X‐ray diffraction experiments with synchrotron radiation show the existence of another modification or of yet unknown decomposition products. The phase transformation from the orthorhombic to the tetragonal polymorph is completely finished at 100 °C. The second effect is detected at 319 °C. 相似文献
10.
PdSCl, a Molecular Palladium(II) Disulfidechloride with Octanuclear Pd8(S2)4Cl8 Groups and with Tetra Metal-coordinated bridging Disulfide Groups Black crystals of PdSCl have been obtained by reaction of Pd with S2Cl2 in closed quartz ampoules at 200°C. The compound is to be formulated as a Palladium(II)-disulfidechloride consisting of Pd8(S2)4Cl8 molecules with approximately D4h symmetry. In the octanuclear complexes Pd atoms form a cube, where bridging disulfide groups are found in front of 4 faces and μ2?bridging Cl atoms on 8 edges. In the monoclinic crystal structure (a = 8.763(2) Å; b = 9.082(2) Å; c = 13.662(4) Å; β = 91.748(23)°; V = 1086.8 Å3; Z = 16 PdSCl; Space gr. P21/n) the molecules form a cubic closed arrangement. 相似文献
11.
Robert Glaum 《无机化学与普通化学杂志》1992,616(10):46-52
Contributions on the Thermal Behaviour of Anhydrous Phosphates. IX. Synthesis and Crystal Structure of Cr6(P2O7)4. A Pyrophosphate Containing Di- and Trivalent Chromium Cr6(P2O7)4 (Cr22+Cr43+(P2O7)4) can be obtained reducing CrPO4 by phosphorus (950°C, 48 h, 100 mg iodine as mineralizer). By means of chemical transport reactions (transport agent iodine; 1050 → 950°C) the compound has been separated from its neighbour phases (Cr2P2O7, CrP3O9) and crystallized (greenish, transparent crystals; edge length up to 0.3 mm). The crystal structure of Cr6(P2O7)4 (Spcgrp.: P-1; z = 1; a = 4.7128(8) Å, b = 12.667(3) Å, c = 7.843(2) Å, α = 89.65(2)°, β = 92.02(2)°, γ = 90.37(2) has been solved and refined from single crystal data (2713 unique reflections, 194 parameter, R = 0.035). Cr2+ is surrounded by six oxygen atoms which occupy the corners of an elongated octahedron (4 × dCr? O ≈? 2.04 Å; 2 × dCr? O ≈? 2.62 Å). The Cr3+ ions are also coordinated octahedraly (1.930 Å ≤ dCr? O ≤ 2.061 Å). The crystallographically independent pyrophosphate groups show nearly eclipsed conformation. The bridging angles (P? O? P) are 136.5° and 138.9° respectively. 相似文献
12.
Tl4Pd3Cl10 – A Compound with a New [(PdCl2Cl2/2)4]4– Group Single crystals of Tl4Pd3Cl10 can be obtained by hydrothermal synthesis. They show tetragonal symmetry with lattice parameters a = 15.956(1) Å and c = 14.146(1) Å, Z = 8 and space group I42d (No. 122). The atomic arrangement of Tl4Pd3Cl10 is explored by X‐ray crystal structure analysis. Tl4Pd3Cl10 is the first example of a new structural type with a hitherto not isolated tetramer [(PdCl2Cl2/2)4]4– group. 相似文献
13.
Six polynuclear chlorobismuthates are formed in the reaction between BiCl3 and Ph4PCl by variation of the molar ratio of the educts, the solvents and the crystallisation methods: [Ph4P]3[Bi2Cl9] · 2 CH2Cl2, [Ph4P]3[Bi2Cl9] · CH3COCH3, [Ph4P]2[Bi2Cl8] · 2 CH3COCH3, [Ph4P]4[Bi4Cl16] · 3 CH3CN, [Ph4P]4[Bi6Cl22], and [Ph4P]4[Bi8Cl28]. We report the crystal structure of [Ph4P]3[Bi2Cl9] · 2 CH2Cl2 which crystallises with triclinic symmetry in the S. G. P1 No. 2, with the lattice parameters a = 13.080(3) Å, b = 14.369(3) Å, c = 21.397(4) Å, α = 96.83(1)°, β = 95.96(1)°, γ = 95.94(2)°, V = 3943.9(1) Å3, Z = 2. The anion is formed from two face‐sharing BiCl6‐octahedra. [Ph4P]2[Bi2Cl8] · 2 CH3COCH3 crystallises with monoclinic symmetry in the S. G. P21/n, No. 14, with the lattice parameters a = 14.045(5) Å, b = 12.921(4) Å, c = 17.098(3) Å, β = 111.10(2)°, V = 2894.8(2) Å3, Z = 2. The anion is a bi‐octahedron of two square‐pyramids, joined by a common edge. The octahedral coordination is achieved with two acetone ligands. [Ph4P]4[Bi4Cl16] · 3 CH3CN crystallises in the triclinic S. G., P1, No. 2, with the lattice parameters a = 14.245(9) Å, b = 17.318(6) Å, c = 24.475(8) Å, α = 104.66(3)°, β = 95.93(3)°, γ = 106.90(4)°, V = 5486(4) Å3, Z = 2. Two Bi2Cl8 dimers in syn‐position form the cubic anion. Lattice parameters of [Ph4P]3[Bi2Cl9] · CH3COCH3 are also given. The solvated compounds are desolvated at approximately 100 °C. [Ph4P]3[Bi2Cl9] · 2 CH2Cl2 and [Ph4P]3[Bi2Cl9] · CH3COCH3 show the same sequence of phase transitions after desolvation. All compounds melt into a liquid in which some order is observed and transform on cooling into the glassy state. 相似文献
14.
The pale‐rose compound [(μ‐C6H8O4)4/2Co(μ‐H2O)2Co(H2O)4] · 4 H2O was prepared from adipic acid and CoCO3 in aqueous solution. The crystal structure (monoclinic, P21/n (no. 14), a = 8.061(1), b = 15.160(2), c = 9.708(2) Å, β = 90.939(7)°, Z = 2, R = 0.0405, wR2 = 0.0971) consists of adipate bridged supramolecular [(μ‐C6H8O4)4/2Co(μ‐H2O)2Co(H2O)4] layers and hydrogen bonded H2O molecules. The cobalt atoms Co1 and Co2 are distorted octahedrally coordinated by the O atoms of two bridging trans‐H2O molecules and four bidentate adipate anions (Co1) and by the O atoms of two bridging trans‐H2O molecules and four monodentate H2O molecules (Co2), respectively. Equatorial bonds: d(Co1–O) = 2.048 Å (2 × ), 2.060 Å (2 × ); d(Co2–O) = 2.057 Å (2 × ), 2.072 Å (2 × ). Axial bonds: d(Co1–O) = 2.235 Å (2 × ); d(Co2–O) = 2.156 Å (2 × ). 相似文献
15.
The crystal structure of bis(semicarbazido)copper(II) nitrate [Cu(NH2NHC(O)NH2)2](NO3)2 has been studied by X-ray diffraction. Monoclinic crystals, a = 6.835(2) Å, b = 7.733(2) Å, c = 10.320(3) Å, β = 105.701(3)°, V = 525.1(2) Å3, space group P21/c, Z = 2, d
msd = 2.136 g/cm3, μ(MoK
α) = 2.143 mm−1. The structure was solved with the program for automatic analysis of Patterson’s function and refined by full-matrix least
squares in an anisotropic approximation for all non-hydrogen atoms using 753 independent reflections; R
1 = 0.0203. The square environment of the Cu atom is formed from the amino nitrogen atoms of the hydrazine fragments and the
C=O oxygen atoms of the two semicarbazide bidentate molecules (Cu-N 1.928 Å, Cu-O 1.999 Å). The axial positions are occupied
by the O atoms of the NO
3
−
outer-spheric anions (Cu-O 2.505 Å). In the structure, the complex cations and the NO
3
−
anions are linked into a framework by N-H...O type hydrogen bonds.
Original Russian Text Copyright ? 2007 by G. V. Romanenko, Z. A. Savelieva, and S. V. Larionov
__________
Translated from Zhurnal Strukturnoi Khimii, Vol. 48, No. 2, pp. 370–373, March–April, 2007. 相似文献
16.
A. Leineweber H. Jacobs R. Eßmann P. Allenspach F. Fauth P. Fischer 《无机化学与普通化学杂志》2001,627(9):2063-2069
Diammine cobalt(II) chloride, Co(N(H, D)3)2Cl2 was prepared by decomposition of the corresponding hexaammines at 120 °C in dynamical vacuum. Crystal structures and magnetic properties of these materials were characterised by X‐ray and neutron powder diffraction, and heat capacity measurements. At ambient temperatures Co(N(H, D)3)2Cl2 crystallises in the Cd(NH3)2Cl2 type structure: space group Cmmm, Z = 2, a = 8.0512(2) Å, b = 8.0525(2) Å, c = 3.73318(9) Å (X‐ray data of the H compound). This structure consists of chains of edge‐sharing octahedra [CoCl4/2(NH3)2] running along the c‐axis. Neutron diffraction confirms that that the ND3 groups are rotationally disordered at ambient temperatures. At 1.5 K and 20 K neutron diffraction data reveal rotational ordering of the ND3 groups leading to doubling of the c‐axis and to Ibmm symmetry: a = 7.9999(6) Å, b = 7.9911(5) Å, c = 7.4033(3) Å (Z = 4, values for T = 1.5 K). Furthermore, antiferromagnetic ordering is present at these temperatures. It is caused by a ferromagnetic coupling of the magnetic moments at Co2+ (3.60(5) μB at 1.5 K, 3.22(5) μB at 20 K) along the octahedra chains [CoCl4/2(NH3)2] and antiferromagnetic coupling between neighbouring chains. According to heat capacity measurements the phase transition antiferromagnetic‐paramagnetic takes place at TN = 26 K. 相似文献
17.
Blue crystals of a Cu(NO3)2 · H2O were synthesized by interaction of CuO with boiling 100% HNO3. Stable β-Cu(NO3)2 modification was obtained by the sublimation of copper(II) nitrate in evacuated ampoule over the 150→100°C temperature gradient for 24 hr. According to X-Ray single crystal analysis Cu(NO3)2 · H2O is monoclinic with a = 6.377(1), b = 8.548(1), c = 9.769(1) Å, β = 100.41(1)°, Z = 4, and space group P21/c. β-modification Cu(NO3)2 is orthorhombic with a = 14.161(5), b = 7.516(3), c = 12.886(2) Å, Z = 12, and space group Pbcn. In the both structures Cu atoms are square coordinated by 4 O atoms at the distances ranging from 1.92 to 2.02 Å. In each structure there are also additional Cu? O bonds with the distance of 2.33 or 2.35 Å and some weaker ones with the distances in the range of 2.65–2.72 Å. In the Cu(NO3)2 · H2O structure the [CuO4] squares are connected by the bridging NO3 groups into zigzag chains, which are linked into layers by the longer Cu? O bonds. In the β-Cu(NO3)2 structure the [CuO4] fragments of two types are joined by the bridging NO3 groups in a three-dimensional framework. Some correlations were found between N? O distances and coordination functions of O atoms. 相似文献
18.
Pb2PdX6 (X = Cl, Br) – Compounds with Elongated [PdX6] Octahedra In contradiction to published data new compounds in the systems PbX2—PdX2 (X = Cl, Br) with the formula Pb2PdCl6 (I) and Pb2PdBr6 (II) were found. These were synthesized by thermal treatment of the corresponding mixtures of PbX2 and PdX2 (X = Cl, Br). X-ray single crystal structure analysis shows isotypism of I and II, monoclinic, P21/c (No. 14), Z = 2, I: a = 9.037(2) Å, b = 6.224(1) Å, c = 8.162(1) Å, β = 90.31(7)β, II: a = 9.512(7) Å, b = 6.584(8) Å, c = 8.383(3) Å, β = 90.07(5)º. Strongly elongated PdX6 octahedra are found in the crystal structure. Additional characterisation of the compounds was done by DTA, IR/RAMAN spectra and 207Pb MAS NMR investigations. Remarcable low field shifts were found for 207Pb. 相似文献
19.
The blue copper complex compounds [Cu(phen)2(C6H8O4)] · 4.5 H2O ( 1 ) and [(Cu2(phen)2Cl2)(C6H8O4)] · 4 H2O ( 2 ) were synthesized from CuCl2, 1,10‐phenanthroline (phen) and adipic acid in CH3OH/H2O solutions. [Cu(phen)2‐ (C6H8O4)] complexes and hydrogen bonded H2O molecules form the crystal structure of ( 1 ) (P1 (no. 2), a = 10.086(2) Å, b = 11.470(2) Å, c = 16.523(3) Å, α = 99.80(1)°, β = 115.13(1)°, γ = 115.13(1)°, V = 1617.5(5) Å3, Z = 2). The Cu atoms are square‐pyramidally coordinated by four N atoms of the phen ligands and one O atom of the adipate anion (d(Cu–O) = 1.989 Å, d(Cu–N) = 2.032–2.040 Å, axial d(Cu–N) = 2.235 Å). π‐π stacking interactions between phen ligands are responsible for the formation of supramolecular assemblies of [Cu(phen)2(C6H8O4)] complex molecules into 1 D chains along [111]. The crystal structure of ( 2 ) shows polymeric [(Cu2(phen)2Cl2)(C6H8O4)2/2] chains (P1 (no. 2), a = 7.013(1) Å, b = 10.376(1) Å, c = 11.372(3) Å, α = 73.64(1)°, β = 78.15(2)°, γ = 81.44(1)°, V = 773.5(2) Å3, Z = 1). The Cu atoms are fivefold coordinated by two Cl atoms, two N atoms of phen ligands and one O atom of the adipate anion, forming [CuCl2N2O] square pyramids with an axial Cl atom (d(Cu–O) = 1.958 Å, d(Cu–N) = 2.017–2.033 Å, d(Cu–Cl) = 2.281 Å; axial d(Cu–Cl) = 2.724 Å). Two square pyramids are condensed via the common Cl–Cl edge to centrosymmetric [Cu2Cl2N4O2] dimers, which are connected via the adipate anions to form the [(Cu2(phen)2Cl2)(C6H8O4)2/2] chains. The supramolecular 3 D network results from π‐π stacking interactions between the chains. H2O molecules are located in tunnels. 相似文献
20.
Transparent yellow crystals of Ba4[WN4]Cl2 were grown at 850°C by the reaction of Ba(NH2)2 with W in a KCl melt under flowing nitrogen. The compound crystallizes monoclinic in P21/m and Z = 2 with the cell parameters a = 8.447(4) Å, b = 6.143(2) Å, c = 10.727(6) Å and β = 99.04(4)°. The crystal structure contains isolated anions [WN4]6? and Cl?. It is the first nitridotungstate(VI) chloride reported so far. 相似文献