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1.
Orange needles of BaEr2S4 are obtained during an investigation of the Ba/Er/U/S system by solid state reaction of a mixture of 238U, Er, BaS, and S in the ratio 1:1:3:3 (evacuated C‐coated fused silica tube, 1273 K, 8 d, cooling rate 3 K/h) together with black crystals of Sb2S3 and US2.  相似文献   

2.
Colorless lath-shaped single crystals of the title compound are obtained from a melt of Y2O3, YF3, and SiO2 (2:5:3 molar ratio) using CsCl as a flux (evacuated silica tube, 973 K, 9 d, 10 K/h cooling rate).  相似文献   

3.
The title compounds are obtained quantitatively by reacting mixtures of M2O3 (M: Fe, In), H3BO3, and NH4H2PO4 in a molar ratio of 1:1:3 at 1153 K.  相似文献   

4.
Crystal Structure of the Isothiocyanato Complex [Ph3PNH2(OEt2)][Sm(NCS)4(DME)2] Colourless single crystals of [Ph3PNH2(OEt2)][Sm(NCS)4(DME)2] ( 1 ) have been obtained besides of Ph3PS from the reaction of the homoleptic phosphorane iminato complex [Sm(NPPh3)3]2 with carbon disulfide in THF solution, followed by recrystallisation from DME/Et2O. According to the crystal structure analysis 1 consists of [Ph3PNH2]+ cations with the diethylether molecule forming a N–H…O hydrogen bridge, and anions [Sm(NCS)4(DME)2]. Sm3+ realizes coordination number eight by four nitrogen atoms of the isothiocyanato ions and by four oxygen atoms of the DME chelates. 1 : Space group P 1, Z = 4, lattice dimensions at 193 K: a = 919.0(1), b = 1965.2(2), c = 2401.3(2) pm, α = 96.748(11)°, β = 94.827(10)°, γ = 91.720(11)°, R = 0.029.  相似文献   

5.
Synthesis and Structure of Tetrafluoroaurates(III) MI[AuF4] with MI = Li, Rb Single crystal investigations on Rb[AuF4], light yellow, confirm the tetragonal unit cell (K[BrF4]-type) with a = 618.2(1) and c = 1191(1) pm, Z = 4, space group I 4/mcm-D (No. 140). Li[AuF4], light yellow too, crystallizes monoclinic with a = 485.32(7), b = 634.29(8), c = 1004.43(13) pm, β = 92.759(12), Z = 4; space group P 2/c-C (No. 13). The structure of Li[AuF4] is related to the Rb[AuF4]-type of structure.  相似文献   

6.
Reaction of cobalt(II) chloride hexahydrate with N‐substituted diethanolamines H2L2–4 ( 3 ) in the presence of LiH in anhydrous THF leads under anaerobic conditions to the formation of three isostructural tetranuclear cobalt(II) complexes [CoII4(Cl)4(HL2–4)4] ( 4 ) with a [Co43‐O)4]4+ cubane core. According to X‐ray structural analyses, the complexes 4 a , c crystallize in the tetragonal space group I41/a, whereas for complex 4 b the tetragonal space group P$\bar 4$ was found. In the solid state the orientation of the cubane cores and the formation of a 3D framework were controlled by the ligand substituents of the cobalt(II) cubanes 4 . This also allowed detailed magnetic investigations on single crystals. The analysis of the SQUID magnetic susceptibility data for 4 a gave intramolecular ferromagnetic couplings of the cobalt(II) ions (J1≈20.4 K, J2≈7.6 K), resulting in an S=6 ground‐state multiplet. The anisotropy was found to be of the easy‐axis type (D=?1.55 K) with a resulting anisotropy barrier of Δ≈55.8 K. Two‐dimensional electron‐gas (2DEG) Hall magnetization measurements revealed that complex 4 a is a single‐molecule magnet and shows hysteretic magnetization characteristics with typical temperature and sweep‐rate dependencies below a blocking temperature of about 4.4 K. The hysteresis loops collapse at zero field owing to fast quantum tunneling of the magnetization (QTM). The structural and electronic properties of cobalt(II) cubane 4 a , deposited on a highly oriented pyrolytic graphite (HOPG) surface, were investigated by means of STM and current imaging tunneling spectroscopy (CITS) at RT and standard atmospheric pressure. In CITS measurements the rather large contrast found at the expected locations of the metal centers of the molecules indicated the presence of a strongly localized LUMO.  相似文献   

7.
Polycrystalline gaudefroyite‐type YCa3(CrO)3(BO3)4 with Cr3+ ions (3d3, S = 3/2) forming an undistorted Kagome lattice is prepared by reaction of a stoichiometric mixture of Y2O3, CaCO3, Cr2O3, H3BO3 in a KCl flux (Al2O3 crucible, 1000 °C, 1 d) followed by re‐grinding and further annealing (1000 °C, 2 d, 95% yield).  相似文献   

8.
New Phosphorus-bridged Transition Metal Carbonyl Complexes. The Crystal Structures of [Re2(CO)7(PtBu)3], [Co4(CO)10(PtBu)2], [Ir4(CO)6(PtBu)6], and [Ni4(CO)10(PiPr)6], (PtBu)3 reacts with [Mn2(CO)10], [Re2(CO)10], [Co2(CO)8] and [Ir4(CO)12] to form the multinuclear complexes [M2(CO)7(PtBu)3] (M = Re ( 1 ), Mn ( 5 )), [Co4(CO)10(PtBu)2] ( 2 ) and [Ir4(CO)6(PtBu)6] ( 3 ). The reaction of (PiPr)3 with [Ni(CO)4] leads to the tetranuclear cluster [Ni4(CO)10(PiPr)6] ( 4 ). The complex structures were obtained by X-ray single crystal structure analysis: ( 1 : space group P1 (Nr. 2), Z = 2, a = 917.8(3) pm, b = 926.4(3) pm, c = 1 705.6(7) pm, α = 79.75(3)°, β = 85.21(3)°, γ = 66.33(2)°; 2 : space group C2/c (Nr. 15), Z = 4, a = 1 347.7(6) pm, b = 1 032.0(3) pm, c = 1 935.6(8) pm, β = 105.67(2)°; 3 : space group P1 (Nr. 2), Z = 4, a = 1 096.7(4)pm, b = 1 889.8(10)pm, c = 2 485.1(12) pm, α = 75.79(3)°, β = 84.29(3)°, γ = 74.96(3)°; 4 : space group P21/c (Nr. 14), Z = 4, a = 2 002.8(5) pm, b = 1 137.2(8) pm, c = 1 872.5(5) pm, β = 95.52(2)°).  相似文献   

9.
Crystal Chemistry of the Lead Lanthanide Oxoaluminates. On Pb2HoAl3O8 and Pb2LuAl3O8 . Single crystals of (I) Pb2HoAl3O8 and (II) Pb2LuAl3O8 were prepared by flux technique and investigated by X-ray methods. It crystallizes with cubic symmetry, space group O–P42/n 3 2/m, (I): a = 9.4164(13) Å, (II): a = 9.3486(8) Å, Z = 4. The new structure type shows AlO4 tetrahedra, LnO8 hexagonal bipyramids and one sided coordinated Pb2+ within heterocubane units. The crystal chemical relationships to other lead oxides containing heterocubane Pb4O4 units are discussed.  相似文献   

10.
Syntheses and Crystal Structures of [Pd9As8(PPh2)8] and [Pd9Sb6(PPh3)8] [PdCl2(PPh3)2] reacts with As(SiMe3)3 to give the new cluster [Pd9As8(PPh3)8] ( 4 ). 4 has been characterized by X-ray crystal structure analysis. It is a molecule in which four [Pd2(PPh3)2]-units are bridged by As2-units. A further Pd atom is located in the centre of the cluster. 4 crystallizes in the space group C2/c with four formula units per unit cell. The lattice constants at 200 K are: a = 3 970.6(3), b = 1 648.90(16), c = 3 266.30(20) pm, β = 131,44(4)°. The reaction of [PdCl2(PPh3)2] with Sb(SiMe3)3 yields [Pd9Sb6(PPh3)8] ( 5 ). 5 consists of a body centred cubic Pd9-cluster. All of the cube faces are capped by μ4-Sb-ligands. 5 crystallizes in the space group Pn3 with two formula units per unit cell. The lattice constants at 200 K are: a = b = c = 1 995.4(2) pm.  相似文献   

11.
On a New Copper Cobalt Borate Oxide with Isolated B2O5 Units: Cu2Co(B2O5)O Single crystals of a new compound with the empirical formula Cu2CoB2O6 were obtained by using a B2O3 flux technique. X-ray single crystal technique led to a new structure type. Cu2CoB2O6 crystallizes monoclinic, space group C-P21/c (No. 14); a = 3.2250(6); b = 14.847(1); c = 9.1171(6) Å; β = 93.67°; Z = 4. All metal sites are octahedrally coordinated and form a two dimensional framework consisting of edge sharing octahedra ribbons. In addition one observes isolated B2O5-units and oxygen which is not coordinated to boron. The far relation to the crystal structure of the mineral Warwickite is illustrated.  相似文献   

12.
The Crystal Structure of KGaO2 and NaGaO2(II) By annealing intimate mixtures of K2O, Na2O and β-Ga2O3 (K : Na : Ga = 2.2 : 1.1 : 1) we obtained single crystals of K2Na4[(GaO3)2] and KGaO2 (Ag-cylinder; 600°C, 26 d). Structure refinement for KGaO2 (four-circle diffractometer data, Mo-Kα , 1 390 or 1 390 Io(hkl); R = 5.55%, Rw = 3.05%) confirms the space group Pbca; a = 552.1 pm, b = 1 107.5 pm, c = 1 580.7 pm, Z = 16. According to K[GaO4/2] we have a stuffed cristobalite-related structure. Single crystals of NaGaO2(II) were grown by annealing intimate mixtures of Na2O2 and GaAs (Na2O2 : GaAs 4.1 : 1) in Ag-cylinders that were not completely closed (570°C, 6 weeks). Structure refinement for NaGaO2(II) (four-circle diffractometer data, Mo-Kα , 588 of 616 Io(hkl); R = 4.54%, Rw = 4.06%) confirms the spacegroup Pna21; a = 549.8(1) pm, b = 720.6(1) pm, c = 529.8(1) pm, Z = 4. In NaGaO2(II) we have a wurtzite-related structure.  相似文献   

13.
Synthesis and Structure of the Phosphorus-bridged Transition Metal Complexes [Fe2(CO)6(PR)6] (R = tBu, iPr), [Fe2(CO)4(PiPr)6], [Fe2(CO)3Cl2(PtBu)5], [Co4(CO)10(PiPr)3], [Ni5(CO)10(PiPr)6], and [Ir4(C8H12)4Cl2(PPh)4] (PtBu)3 and (PiPr)3 react with [Fe2(CO)9] to form the dinuclear complexes [Fe2(CO)6(PR)6] (R = tBu: 1 ; iPr: 2 ). 2 is also formed besides [Fe2(CO)4(PiPr)6] ( 3 ) in the reaction of [Fe(CO)5] with (PiPr)3. When PiPr(PtBu)2 and PiPrCl2 are allowed to react with [Fe2(CO)9] it is possible to isolate [Fe2(CO)3Cl2(PtBu)5] ( 4 ). The reactions of (PiPr)3 with [Co2(CO)8] and [Ni(CO)4] lead to the tetra- and pentanuclear clusters [Co4(CO)10(PiPr)3] ( 5 ), [Ni4(CO)10(PiPr)6] [2] and [Ni5(CO)10(PiPr)6] ( 6 ). Finally the reaction of [Ir(C8H12)Cl]2 with K2(PPh)4 leads to the complex [Ir4(C8H12)4Cl2(PPh)4] ( 7 ). The structures of 1–7 were obtained by X-ray single crystal structure analysis (1: space group P21/c (Nr. 14), Z = 8, a = 1 758.8(16) pm, b = 3 625.6(18) pm, c = 1 202.7(7) pm, β = 90.07(3)°; 2 : space group P1 (Nr. 2), Z = 1, a = 880.0(2) pm, b = 932.3(3) pm, c = 1 073.7(2) pm, α = 79.07(2)°, β = 86.93(2)°, γ = 72.23(2)°; 3 : space group Pbca (Nr. 61), Z = 8, a = 952.6(8) pm, b = 1 787.6(12) pm, c = 3 697.2(30) pm; 4 : space group P21/n (Nr. 14), Z = 4, a = 968.0(4) pm, b = 3 362.5(15) pm, c = 1 051.6(3) pm, β = 109.71(2)°; 5 : space group P21/n (Nr. 14), Z = 4, a = 1 040.7(5) pm, b = 1 686.0(5) pm, c = 1 567.7(9) pm, β = 93.88(4)°; 6 : space group Pbca (Nr. 61), Z = 8, a = 1 904.1(8) pm, b = 1 959.9(8) pm, c = 2 309.7(9) pm. 7 : space group P1 (Nr. 2), Z = 2, a = 1 374.4(7) pm, b = 1 476.0(8) pm, c = 1 653.2(9) pm, α = 83.87(4)°, β = 88.76(4)°, γ = 88.28(4)°).  相似文献   

14.
Sulfide Chlorides (MSCl) of the Light Lanthanides (M = La–Pr) The reactions of the light lanthanides (M = La–Nd) with sulfur and the respective trichlorides (MCl3) in evacuated silica tubes (850 °C, 7 d) yield single-phase sulfide chlorides of the composition MSCl when appropriate molar ratios (2 : 3 : 1) of the reactants (M : S : MCl3) are used. A slight excess of trichloride as a flux promotes the formation of lath-shaped transparent single crystals (colorless for M = La and Ce, apple-green for M = Pr) which prove to be water soluble and sensitive to hydrolysis. The crystal structure was determined from X-ray single-crystal data taking LaSCl (orthorhombic, Pbcm (no. 57), a = 680.22(5), b = 705.26(7), c = 4203.7(3) pm, Z = 24, R = 0.069, Rw = 0.043) as an example. According to Guinier powder data CeSCl and quickly quenched samples of PrSCl crystallize isotypically. Thus four crystallographically independent cations (M3+) are present, each coordinated by four S2– but differing in the number of their next Cl neighbors. The figures of coordination are completed by four Cl about M1 (square antiprism, CN = 8), by only two Cl about M2 (trigonal prism, CN = 6), and by three Cl each about M3 and M4 (capped trigonal prisms, CN = 7). Six crystallographically different anions, although indistinguishable by X-ray diffraction, exhibit coordination numbers of four (S2–, 3 ×) and three (Cl, 3 ×) with respect to the cations. So PbO-analogous layers of the composition [SM4/4]+ parallel (100) are formed and held together along [100] by alternatingly sheathed Cl layers.  相似文献   

15.
Single crystals of the title compounds are prepared by solid state reactions of M2CO3 (M: K, Rb, Cs), PbO, PbF2, H3BO3, and (NH4)H2PO4 in a molar ratio of 2:5:5:4:3 (Pt crucible, 700 °C, 10 h).  相似文献   

16.
Azido Complexes of Vanadium(IV) and Vanadium(V): (Ph4P)2[VOCl2(μ‐N3)]2 and (Ph4P)2[VOCl(μ‐N3)(N3)2]2 (Ph4P)2[VOCl2(μ‐N3)]2 ( 1 ) was prepared by reaction of (Ph4P)[VO2Cl2] with trimethylsilylazide in the molar ratio 1:2 in dichloromethane solution to give dark green, moisture sensitive, non‐explosive single crystals. The reaction is accompanied by the formation of the dark blue side‐product (Ph4P)2[VOCl(μ‐N3)(N3)2]2 ( 2a ), which can be obtained as the main product by application of a large excess of Me3SiN3. Dark blue needles of 2a crystallize spontaneously from the CH2Cl2 solution within one hour at 4 °C. After standing at 4 °C under its mother liquid within 24 hours a first‐order phase transition of 2a occurs forming dark blue prismatic single crystals of 2b . According to single crystal X‐ray structure determinations, 2a and 2b crystallize in the same type of space group , however, with different lattice dimensions. The vanadium(IV) complex 1 is characterized by X‐ray structure determination and by vibrational spectroscopy (IR, Raman) as well as by EPR spectroscopy, whereas 2b is characterized by IR spectroscopy. 1 : Space group P21/n, Z = 2, a = 1009.5(1), b = 1226.6(2), c = 1943.0(2) pm, β = 98.42(1)°, R1 = 0.0672. The complex anion forms centrosymmetric units with V2N2‐four‐membered rings with a V···V distance of 335.6(1) pm and coordination number five on the vanadium(IV) atoms. 2a : Space group , Z = 1, a = 1089.0(2), b = 1097.1(2), c = 1310.1(2) pm, α = 92.99(1)°, β = 106.12(2)°, γ = 117.05(2)°, V = 1309.8(4) Å3, dcalc. = 1.440 g·cm?3, R1 = 0.0384. The complex anion forms centrosymmetric units of symmetry Ci with V2N2 four‐membered rings and VN bond lengths of 200.4(3) and 234.4(2) pm, respectively. The non‐bonding V···V distance amounts to 356.2(1) pm. 2b : Space group , Z = 1, a = 1037.3(2), b = 1157.6(2), c = 1177.2(2) pm, α = 98.48(2)°, ° = 103.82(2)°, γ = 106.33(2)°, V = 1281.8(4) Å3, dcalc. = 1.471 g·cm?3, R1 = 0.0724. The structure of the complex anion is similar to the anion of 2a with VN bond lengths of the four‐membered V2N2 ring of 203.3(4) and 235.2(4) pm, respectively, and a non‐bonding V···V distance of 357.5(1) pm.  相似文献   

17.
On a New Copper Tin Borate Oxide with Isolated BO3 Units: Cu5Sn(BO3)2O4 Single Crystals of the new compound Cu5Sn(BO3)2O4 were obtained by a B2O3 fluxtechnique. They crystallize in a monoclinic distorted variant of a Ludwigite structure with a partly ordered metal distribution. X-ray investigations on single crystals led to the space group C–P21/c (No. 14); a = 6.3526(7); b = 9.502(1); c = 12.100(9) Å; β = 93.30(3)°; Z = 4. All metal-sites are distorted octahedraly coordinated by oxygen-ions. The structure contains BO3-units and oxygen which is not coordinated to boron.  相似文献   

18.
Crystal Structure of KZr2(AsO4)3 KZr2(AsO4)3 crystals have been prepared by the flux method. The compound crystallizes in the rhombohedral system with the parameters: a = 9.028(1), c = 24.399(3) Å. The density is d = 3.694 g/cm3 and Z = 6. The space group is R3 c. The structure has been solved by isotypism with that of NaZr2(PO4)3 to R = 0.041, for 353 independent reflections. It consists in 3-dimensional chains of AsO4 tetrahedra and ZrO6 octahedra. K+ ions are the center of the antiprism with K—O distances equal to 2.813 Å. The Zr–O and As–O distances have the same values of those usually observed (Zr–O = 2,05 Å and As–O = 1.66 Å).  相似文献   

19.
Crystal structures and electrical properties of radical-cation salts of the chiral organic donor TMET (S,S,S,S,-bis-(dimethylethylenedithio)tetrathiafulvalene) are described. Two structural types, 2:1 with octahedral anions Pf, AsF, SbF, I (incommensurate), and 3:2 with tetrahedral anions BF?4, CIO?4, ReO?4 are observed. Resistivity measurements between 2 and 298 K indicate that the 3:2 types are organic metals, while the other compounds are semiconductors. (TMET)3(CIO4)2 is metallic down to about 120 K at ambient pressure and remains metallic down to 2 K at 8 kbar.  相似文献   

20.
Three new 3D metal-organic porous frameworks based on Co(II) and 2,2′-bithiophen-5,5′-dicarboxylate (btdc2−) [Co3(btdc)3(bpy)2]·4DMF, 1; [Co3(btdc)3(pz)(dmf)2]·4DMF·1.5H2O, 2; [Co3(btdc)3(dmf)4]∙2DMF∙2H2O, 3 (bpy = 2,2′-bipyridyl, pz = pyrazine, dmf = N,N-dimethylformamide) were synthesized and structurally characterized. All compounds share the same trinuclear carboxylate building units {Co3(RCOO)6}, connected either by btdc2– ligands (1, 3) or by both btdc2– and pz bridging ligands (2). The permanent porosity of 1 was confirmed by N2, O2, CO, CO2, CH4 adsorption measurements at various temperatures (77 K, 273 K, 298 K), resulted in BET surface area 667 m2⋅g−1 and promising gas separation performance with selectivity factors up to 35.7 for CO2/N2, 45.4 for CO2/O2, 20.8 for CO2/CO, and 4.8 for CO2/CH4. The molar magnetic susceptibilities χp(T) were measured for 1 and 2 in the temperature range 1.77–330 K at magnetic fields up to 10 kOe. The room-temperature values of the effective magnetic moments for compounds 1 and 2 are μeff (300 K) ≈ 4.93 μB. The obtained results confirm the mainly paramagnetic nature of both compounds with some antiferromagnetic interactions at low-temperatures T < 20 K in 2 between the Co(II) cations separated by short pz linkers. Similar conclusions were also derived from the field-depending magnetization data of 1 and 2.  相似文献   

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