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1.
Crystal Structure of (NMe4)2[Re3Br11(H2O)] [Re3Br9(H2O)3](H2O)2 . (NMe4)2[Re3Br11(H2O)] [Re3Br9(H2O)3](H2O)2 crystallizes from hydrobromic acid solution of Re3Br9 · 2 H2O and NMe4Br at 0 – 5°C. The crystal structure (monoclinic; P21/m (Nr. 11); a = 967.9(3); b = 1 529.7(4); c = 1 710.9(4) pm; β = 91.66(2)°; Z = 2; R = 0.113; Rw = 0.068) has been determined from four-circle diffractometer data. The structure contains two different cluster units of trivalent rhenium, isolated anionic [Re3Br11(H2O)]2? units and neutral cluster units that are connected through crystal water molecules to chains{[Re3Br9(H2O)3](H2O)2}. 相似文献
2.
H. Imoto N. G. Naumov A. V. Virovets T. Saito V. E. Fedorov 《Journal of Structural Chemistry》1998,39(5):720-727
Crystal structures of Cs4[Re6Te8(CN)6]·2H2O (1) and Ba2[Re6Te8(CN)6]· 12H2O (2) are determined. Crystals 1 are orthorhombic, a = 14,282(1), b = 12.910(1), c = 18.040(1) Å, Vcell = 3326.3(8) Å3, space group Pbcn, Z = 4, dcalc = 5.715 g/cm3, R(F) = 0.0482 for 3193 Fhkl > 4σ(F). Crystals 2 are triclinic, a = 9.671(3), b = 9.697(4), c = 11.039(4) Å, α = 89.86(3), β = 72.34(3), γ = 82.46(3)°, Vcell = 977.2(6) Å3, space group P1, Z = 1, dcalc = 4.733 g/cm3, R(F) = 0.0490 for 3226 Fhkl > 4σ(F). In both structures, the [Re6Te8(CN)6]4? anions form a distorted primitive cubic packing with distances between the centers 9.02-9.63 Å in 1 and 9.70-11.04 Å in 2. The Cs+ cations in 1 lie near the face centers of the cubes formed by the onions. In 2, cation pairs (Ba2+)2 bonded to two solvate water molecules are formed; the pairs lie at the centers of the anion cubes. In structures 1 and 2, there are shortened contacts between the tellurium atoms belonging to the neighboring anions (3.75-4.09 and 3.95-4.22 Å, respectively). 相似文献
3.
4.
Three new strontium vanadium borophosphate compounds, (NH4)2(C2H10N2)6[Sr(H2O)5]2[V2P2BO12]6 10H2O (Sr-VBPO1) (1), (NH4)2(C3H12N2)6[Sr(H2O)4]2[V2P2BO12]6 17H2O (Sr-VBPO2) (2), and (NH4)3(C4H14N2)4.5[Sr(H2O)5]2[Sr(H2O)4][V2P2BO12]6 10H2O (Sr-VBPO3) (3) have been synthesized by interdiffusion methods in the presence of diprotonated ethylenediamine, 1,3-diaminopropane, and 1,4-diaminobutane. Compound 1 has a chain structure, whereas 2 and 3 have layered structures with different arrangements of [(NH4) [symbol: see text] [V2P2BO12]6] cluster anions within the layers. Crystal data: (NH4)2(C2H10N2)6[Sr(H2O)5]2[V2P2BO12]6 10H2O, monoclinic, space group C2/c (no. 15), a = 21.552(1) A, b = 27.694(2) A, c = 20.552(1) A, beta = 113.650(1) degrees, Z = 4; (NH4)2(C3H12N2)6[Sr(H2O)4]2[V2P2BO12]6 17H2O, monoclinic, space group I2/m (no. 12), a = 15.7618(9) A, b = 16.4821(9) A, c = 21.112(1) A, beta = 107.473(1) degrees, Z = 2; (NH4)3(C4H14N2)4.5[Sr(H2O)5]2[Sr(H2O)4] [V2P2BO12]6 10H2O, monoclinic, space group C2/c (no. 15), a = 39.364(2) A, b = 14.0924(7) A, c = 25.342(1) A, beta = 121.259(1) degrees, Z = 4. The differences in the three structures arise from the different steric requirements of the amines that lead to different amine-cluster hydrogen bonds. 相似文献
5.
Bis(dimethylamino)trifluoro sulfonium Salts: [CF3S(NMe2)2]+[Me3SiF2]‐, [CF3S(NMe2)2]+ [HF2]‐ and [CF3S(NMe2)2]+[CF3S]‐ From the reaction of CF3SF3 with an excess of Me2NSiMe3 [CF3(NMe2)2]+[Me3SiF2]‐ (CF3‐BAS‐fluoride) ( 5 ), from CF3SF3/CF3SSCF3 and Me2NSiMe3 [CF3S(NMe2)2]+‐ [CF3S]‐ ( 7 ) are isolated. Thermal decomposition of 5 gives [CF3S(NMe2)2]+ [HF2]‐ ( 6 ). Reaction pathways are discussed, the structures of 5 ‐ 7 are reported. 相似文献
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7.
3硝基1,2,4三唑5酮(NTO)的锂盐水溶液与Yb2O3的稀硝酸溶液反应,制备了标题配合物,其化学式为Yb(NTO)3·10H2O。用X射线衍射法测定配合物的晶体结构,其分子式为[Yb(NTO)3(H2O)4]·6H2O。属单斜晶系,空间群为C2/c。晶胞参数如下:a=36931(5)nm,b=06683(10)nm,c=25656(3)nm,β=130974(5)°,V=47811(11)nm3,Z=8,Dc=2013g·cm-3,μ=4017mm-1,F(000)=2850。镱离子的配位数为7,其配位多面体为五角双锥。 相似文献
8.
Hengbin Zhang Shuyun Niu Guangdi Yang Fu Nie Shujia Li 《Transition Metal Chemistry》1994,19(5):498-502
Summary [Et2N] [Co(NH2CSNHNH2)3] [Mo8O26] ·4Me2NCHO, obtained by reacting MoCl5, CoCl2, thiosemicarbazide and DMF in nonaqueous solvents under i.r. radiation, was characterized by spectroscopy and X-ray crystallography. It contains an octanuclear molydenum anion with two pentabridging oxygen atoms and a cobalt-centred cation bonded to nitrogen and sulphur ligands. 相似文献
9.
A. V. Shtemenko V. G. Stolyarenko K. V. Domasevich 《Russian Journal of Inorganic Chemistry》2006,51(7):1014-1019
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
10.
The 1/2V2O5-H2C2O4/H3PO4/NH4OH system was investigated using hydrothermal techniques. Four new phases, (NH4)VOPO(4).1.5H2O (1), (NH4)0.5VOPO(4).1.5H2O (2), (NH4)2[VO(H2O)3]2[VO(H2O)][VO(PO4)2]2.3H2O (3), and (NH4)2[VO(HPO4)]2(C2O4).H2O (4), have been prepared and structurally characterized. Compounds 1 and 2 have layered structures closely related to VOPO(4).2H2O and A0.5VOPO4.yH2O (A = mono- or divalent metals), whereas 3 has a 3D open-framework structure. Compound 4 has a layered structure and contains both oxalate and phosphate anions coordinated to vanadium cations. Crystal data: (NH4)VOPO(4).1.5H2O, tetragonal (I), space group I4/mmm (No. 139), a = 6.3160(5) A, c = 13.540(2) A, Z = 4; (NH4)0.5VOPO(4).1.5H2O, monoclinic, space group P2(1)/m (No. 11), a = 6.9669(6) A, b = 17.663(2) A, c = 8.9304(8) A, beta = 105.347(1) degrees, Z = 8; (NH4)2[VO(H2O)3]2[VO(H2O)][VO(PO4)2]2.3H2O, triclinic, space group P1 (No. 2), a = 10.2523(9) A, b = 12.263(1) A, c = 12.362(1) A, alpha = 69.041(2) degrees, beta = 65.653(2) degrees, gamma = 87.789(2) degrees, Z = 2; (NH4)2[VO(HPO4)]2(C2O4).5H2O, monoclinic (C), space group C2/m (No. 12), a = 17.735(2) A, b = 6.4180(6) A, c = 22.839(2) A, beta = 102.017(2) degrees, Z = 6. 相似文献
11.
The salts [18-crown-6-K](4)[Sn(4)Se(10)].5en and [18-crown-6-K](4)[Sn(4)Te(10)].3en.2THF were isolated upon addition of THF to the ethylenediamine (en) extracts of the alloys KSn(0.90)Se(1.93) and K(4)Sn(4)Te(10) that had been extracted in the presence of 18-crown-6 (1,4,7,10,13,16-hexaoxacyclooctadecane). The Sn(4)Te(10)(4-) anion has been structurally characterized for the first time by a single-crystal X-ray diffraction study of [18-crown-6-K](4)[Sn(4)Te(10)].3en.2THF: P2(1)/n, a = 22.420(5) A, b = 19.570(4) A, c = 24.680(5) A, beta = 96.90(3)(o), Z = 4, and R(1) = 0.0468 at -183 degrees C. In addition to Si(4)Te(10)(4-) and Ge(4)Te(10)(4-), the Sn(4)Te(10)(4-) anion represents the only other known group 14 adamantanoid telluride. The X-ray crystal structure determination of the related [18-crown-6-K](4)[Sn(4)Se(10)].5en salt has also been determined: P2(1)/n, a = 22.003(2) A, b = 18.966(2) A, c = 24.393(2) A, beta = 97.548(8)(o), Z = 4, and R(1) = 0.0843 at -123 degrees C. The anion geometries are of the adamantanoid type where the Sn(IV) atoms occupy the bridgehead positions and the chalcogen atoms occupy the bridging and terminal sites. The energy minimized geometries of Sn(4)Ch(10)(4-) have also been determined using density functional theory (DFT). Mayer bond order analyses, Mayer valencies, and empirical bond valencies indicate that the terminal Sn-Ch bonds have significant multiple bond character, with the terminal Sn-Se bond having more multiple bond character than the terminal Sn-Te bond. The vibrational frequencies of the Sn(4)Se(10)(4-) and Sn(4)Te(10)(4-) anions have been calculated using DFT methods, allowing the Raman spectrum of Sn(4)Se(10)(4-) to be fully assigned. 相似文献
12.
O. A. Efremova Yu. V. Mironov N. V. Kuratieva V. E. Fedorov 《Russian Chemical Bulletin》2006,55(11):1946-1949
The reactions of the rhenium chalcocyanide cluster salts K4[Re4Q4(CN)12]·6H2O (Q = S or Se) with Cu2+ cations coordinated by the bidentate ligand 2,2′-bipyridyl (bipy) produced two new cluster compounds, [Cu(NH3)(bipy)2]2[Re4S4(CN)12]·bipy·3.25H2O (1) and [{Cu(bipy)2}2Re4Se4(CN)12]·bipy·8.5H2O (2). The structures of these complexes were solved by X-ray diffraction. Compound 1 is ionic. Compound 2 is molecular. In the structures of both compounds, there are staking interactions between the {Cu(bipy)2}2+ cationic moieties and the solvate 2,2′-bipyridyl molecules.
Published in Russian in Izvestiya Akademii Nauk. Seriya Khimicheskaya, No. 11, pp. 1875–1878, November, 2006. 相似文献
13.
Several mixed Te/Se polychalcogenide anions [Te(m)Se(n)](2-) were synthesized at 293 K by reactions between Te(n)(2-)and Se(n)(2-) anions in N,N-dimethylformamide (DMF) in the presence of different-size ammonium or phosphonium cations, in some cases in the presence of metal species. The structures of these anions were determined by single-crystal X-ray diffraction methods. The crystal structures of [NEt(4)](2)[Te(3)Se(6)] (1) and [NEt(4)](2)[Te(3)Se(7)] (2) consist, respectively, of one-dimensional infinite 1(infinity)[Te(3)Se(6)(2-)] and 1(infinity)[Te(3)Se(7)(2-)] anionic chains separated by NEt(4)(+) cations. In compound 1, each chain comprises Te(3)Se(5) eight-membered rings bridged by Se atoms. The Te(3)Se(5) ring has an "open book" conformation. The NMR spectrum of a DMF solution of [NEt(4)](2)[Te(3)Se(6)] crystals at 223 K shows (77)Se resonances at delta = 290, 349, and 771 ppm and a single (125)Te resonance at delta = 944.7 ppm. In compound 2, each chain comprises Te(3)Se(6) five- and six-membered rings bridged by Se atoms. The Te(3)Se(6) ring can be regarded as an inorganic analogue of bicyclononane. The anion of [PPh(4)](2)[Te(2)Se(2)] (4) contains a Se-Te-Te-Se chain with the terminal Se atoms trans to one another. The new compounds [PPN](2)[TeSe(10)] (3), [NMe(4)](2)[TeSe(3)].DMF (5), and [NEt(4)](2)[TeSe(3)] (6) contain known anions. 相似文献
14.
Jovica Stojanovi Tamara ?or?evi Ljiljana Karanovi 《Acta Crystallographica. Section C, Structural Chemistry》2010,66(5):i55-i57
The structure of the title compound, ammineaquadi‐μ5‐phosphato‐trizinc(II), [Zn3(PO4)2(H2O)0.8(NH3)1.2], consists of two parts: (i) PO4 and ZnO4 vertex‐sharing tetrahedra arranged in layers parallel to (100) and (ii) ZnO2(N/O)2 tetrahedra located between the layers. Elemental analysis establishes the ammine‐to‐water ratio as 3:2. ZnO2(N/O)2 tetrahedra are located at special position 4e (site symmetry 2) in C2/c. The two O atoms of ZnO2(N/O)2 are bonded to neighbouring P atoms, forming two Zn—O—P linkages and connecting ZnO2(N/O)2 tetrahedra with two adjacent bc plane layers. A noteworthy feature of the structure is the presence of NH3 and H2O at the same crystallographic position and, consequently, qualitative changes in the pattern of hydrogen bonding and weaker N/O—H...O electrostatic interactions, as compared to two closely related structures. 相似文献
15.
Soheila Chitsaz Dieter Fenske Olaf Fuhr 《Angewandte Chemie (Weinheim an der Bergstrasse, Germany)》2006,118(47):8224-8228
16.
Reaction of C(NMe2)4 with Ni(CO)4 – Syntheses and Structures of [C(NMe2)3][(CO)3NiC(O)NMe2], [C(NMe2)3]2[Ni5(CO)12], and [C(NMe2)3]3[Ni6(CO)12][O2CNMe2] The reaction of C(NMe2)4 with Ni(CO)4 in THF produces the carbamoyl complex [C(NMe2)3][(CO)3NiC(O)NMe2] ( 1 ); side products are the purple cluster compound [C(NMe2)3]2[Ni5(CO)12] · THF ( 2 · THF) and the red cocristallization product [C(NMe2)3]3[Ni6(CO)12][O2CNMe2] ( 3 ). All compounds were studied by X‐ray diffraction analyses. The cations of 3 are all disordered but not those of 1 and 2 . The unit cell of 1 contains two crystallographically independent anions (I and II) which differ in the dihedral angle between the plane of the carbamoyl ligand and the plane defined by the atoms CCarbamoyl–Ni–CO amounting 0° in the anion I and 18° in the anion II. 相似文献
17.
Wang Shutao Wang Enbo Hou Yu Li Yangguang Wang Li Yuan Mei Hu Changwen 《Transition Metal Chemistry》2003,28(6):616-620
A novel organic/inorganic hybrid molybdenum phosphate, [NH3(CH2CH2)2NH3]3[NH3(CH2CH2)2NH2]Na5-[Mo6O12(OH)3(PO4)(HPO4)3]2·4H2O (1), involving molybdenum presented in V oxidation, has been hydrothermally prepared and characterized by elemental analysis, i.r., u.v.–vis., x.p.s., t.g. and single crystal X-ray diffraction. The structure of the title compound (1) may be considered to consist of two [Mo6O12(OH)3(PO4)(HPO4)3] units bonded together with NaO6 octahedra, forming dimers. Further, these dimers connect with each other through four Na+ cations as bridges, giving rise to novel one-dimensional chain-like skeleton. Piperazines exist among inorganic chains acting as charge balancing cations. 相似文献
18.
Masato Hashimoto Michiru Kubata Atsushi Yagasaki 《Acta Crystallographica. Section C, Structural Chemistry》2000,56(12):1411-1412
The title compound, triammonium cis‐diaqua‐cis‐dioxo‐trans‐disulfatovanadate 1.5‐hydrate, was obtained by oxidizing VIV to VV in a 2 M sulfuric acid solution of vanadyl sulfate and adding ammonium sulfate. Here, the V atom is sandwiched by two sulfate groups by corner‐sharing to form a discrete [VO2(SO4)2(OH2)2]3? anion. The water molecules occupy cis positions in the equatorial plane of the vanadium octahedron. 相似文献
19.
New Ni-containing heterometallic cuboidal cluster aqua complex [W3(NiCl)Se4(H2O)9]3+, the missing link in the family of the M3NiQ4 clusters (M = Mo, W; Q = S, Se), has been prepared by the reaction of [W3Se4(H2O)9]4+ with Ni in 2 M HCl. Single crystals of edge-linked double-cuboidal cluster [{W3NiSe4(H2O)9}2](pts)8.18H2O (pts = p-toluenesulfonate) were grown from the solution of the aqua complex in 3 M Hpts, and their structures were determined. The Ni site in the clusters [W3(NiCl)Q4(H2O)9]3+ selectively coordinates typical pi-acceptor ligands such as CO, olefins, acetylenes, phosphines, arsines, or SnCl3-. This allows stabilization by coordination of such elusive species as HP(OH)2 and As(OH)3. The stability constants for coordination of HP(OH)2, As(OH)3, and SnCl3- were determined. The Se for S substitution increases the stability by 1-2 orders of magnitude. Supramolecular adducts with cucurbit[6]uril (Cuc), [W3(Ni(HP(OH)2))Q4(H2O)9]Cl4.Cuc.11H2O and [W3(NiAs(OH)3)S4(H2O)8Cl]Cl3.Cuc.13H2O, were isolated and structurally characterized. 相似文献
20.
Kalinina I. V. Pervukhina N. V. Podberezskaya N. V. Fedin V. P. 《Russian Journal of Coordination Chemistry》2002,28(6):389-393
Single crystals of [Zn(NH3)4]3[Mo4Te4(CN)12] (I) and [Cd(NH3)4]3[W4Te4(CN)12] (II) were obtained by applying solutions of K7[Mo4Te4(CN)12] · 11H2O and K6[W4Te4(CN)12] · 5H2O in aqueous ammonia over solutions of ZnCl2 and Cd(NO3)2 in glycerol and were characterized by X-ray diffraction analysis. The IR spectra and thermal properties of compounds I and II were examined. 相似文献