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1.
Hydrothermal Synthesis and Crystal Structures of Na2Be3(SeO3)4·H2O and Cs2[Mg(H2O)6]3(SeO3)4
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The selenites, Na2Be3(SeO3)4 · H2O and Cs2[Mg(H2O)6]3(SeO3)4, were synthesized under hydrothermal conditions. The crystal structures of Na2Be3(SeO3)4 · H2O and Cs2[Mg(H2O)6]3(SeO3)4 were determined by single‐crystal X‐ray diffractions. Na2Be3(SeO3)4 · H2O crystallizes in the triclinic space group P1 (no. 2) with unit cell parameters a = 4.8493(9), b = 12.013(2), c = 12.077(2) Å, and Z = 2, whereas Cs2[Mg(H2O)6]3(SeO3)4 crystallizes in the monoclinic space group C2/m (no. 12) with lattice cell parameters a = 12.596(6), b = 7.297(4), c = 16.914(8) Å, and Z = 2. Na2Be3(SeO3)4 · H2O features a three‐dimensional open framework structure formed by BeO4 tetrahedra and SeO3 trigonal pyramids. Na cations and H2O molecules are located in different tunnels. Cs2[Mg(H2O)6]3(SeO3)4 has a structure composed of isolated [Mg(H2O)6] octahedra and SeO3 trigonal pyramids interacted by hydrogen bonds, and Cs cations are resided in‐between. Both compounds were characterized by thermogravimetric analysis and FT‐IR spectroscopy. 相似文献
2.
In(OH)(SeO3), prepared by a hydrothermal reaction, crystallizes in a new structure type containing cis InO4(OH)2 octahedra. These groups share both corners (via OH) and edges (via O) to result in a layered motif containing octahedral 8‐ring holes that resembles a single layer of the hollandite structure. The selenium atoms [as pyramidal (SeO3)2? selenite groups] decorate the 8‐ring holes and crosslink the sheets, leading to a three‐dimensional structure. Crystal data: In(OH)(SeO3), Mr = 258.79, triclinic, (No. 2), a = 5.6523 (2) Å, b = 7.9598 (3) Å, c = 8.0911 (3) Å, α = 87.925 (2)°, β = 79.679 (2)°, γ = 83.201 (3)°, V = 355.58 (2) Å3, Z = 4, R (F) = 0.023, wR (F2) = 0.054. 相似文献
3.
The reaction of a mixture of barium and rhenium (3:1) at 850 °C under flowing nitrogen yielded the nitride‐oxide (Ba6O)(ReN3)2 (R (No. 148); a = 8.1178(2) Å, c = 17.5651(4) Å; V = 1002.43(5) Å3; Z = 6). According to a structure refinement on X‐ray powder diffraction data, this compound is isostructural to a recently described nitride‐oxide of osmium of analogous composition. The structure consists of sheets of trigonal ReN3 units and trigonal antiprismatic Ba6O groups. The Ba–O distance of 2.73 Å is close to the sum of the respective ionic radii. The trigonal ReN35– nitride anion displays a Re–N bond length of 1.94 Å, and is planar within the limits of experimental error. The constitution of the anion was confirmed by IR and Raman spectroscopy. The nitride‐oxide is stable up to 1000 °C, semiconducting (σ = 4.57 × 10–3 Ω–1 · cm–1 at RT), and paramagnetic down to 25 K. A Curie–Weiss analysis resulted in a magnetic moment of μ = 0.68 μB per rhenium atom. 相似文献
4.
钴、镍-氨基三乙酸配位聚合物Na[M(nta)]·H2O(M=Co,Ni)的水热合成、结构与磁性 总被引:1,自引:0,他引:1
由有机配体同金属离子作用构建的配位聚合物具有与无机微孔晶体类似的空旷骨架结构,并在非线性光学材料、磁性材料、超导材料及催化等诸多方面具有潜在的应用前景[1~4].在配位聚合物的合成中,配体的种类不仅直接影响到聚合物的合成,而且还涉及到聚合物的结构维数[5~7].目前,用来构建这些配合物的有机配体大多数都带有相同的可配位基团,较少应用具有两种以上的配位基团的有机配体.本文采用同时含有氮和氧两种配位原子的多齿配体氨基三乙酸[8~12],在水热条件下分别以Co2+和Ni2+作为组装基元,通过自组装合成了具有三维骨架结构的Na[M(nta)]·H2O [M=Co(1),Ni(2)]配位聚合物,并进行了结构与磁性研究. 相似文献
5.
Syntheses and Characterization of 1,4‐Phenylenebisphosphonates,A[HO3PC6H4PO3H2] (A = Li,K, Rb,Cs, Tl,Ag and NH4) and Crystal Structure of 1,4‐Phenylenebisphosphonic Acid
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Seven 1,4‐phenylenebisphosphonates of monovalent ions, A(HO3PC6H4PO3H2) (A = Li, K, Rb, Cs, Tl, Ag and NH4), were synthesized and characterized by single‐crystal X‐ray diffraction, spectroscopic and thermal methods. These compounds and the reported sodium analogue have four structure types. The sodium compound, one‐dimensional lithium compound and pillared‐layered cesium compounds have different structure types, whereas the potassium, rubidium, thallium, ammonium and silver compounds have a pillared ladder‐like structure. They undergo initial thermal decomposition in the range of 120–270 °C. Moreover, the single crystal X‐ray structure of 1,4‐phenylenebisphosphonic acid was determined. 相似文献
6.
The new quaternary thiogermanates, ATaGeS5 (A = K, Rb, Cs) were prepared with the use of halide fluxes and the crystal structures of the compounds were determined by single‐crystal X‐ray diffraction methods. The compounds are isostructural and crystallize in space group P\bar{1} of the triclinic system with two formula units in a cell of dimensions: a = 6.937(1) Å, b = 6.950(2) Å, c = 8.844(3) Å, α = 71.07(2)°, β = 78.56(2)°, γ = 75.75(2)°, V = 387.6(2) Å3 for KTaGeS5; a = 6.996(3) Å, b = 7.033(3) Å, c = 8.985(4) Å, α = 70.33(3)°, β = 78.12(4)°, γ = 75.63(4)°, V = 399.6(3) Å3 for RbTaGeS5; a = 7.012(4) Å, b = 7.202(3) Å, c = 9.267(5) Å, α = 68.55(3)°, β = 77.27(4)°, γ = 74.75(4)°, V = 416.2(4) Å3 for CsTaGeS5. The structures of ATaGeS5 (A = K, Rb, Cs) are comprised of anionic infinite two‐dimensional {}_\infty^2 [TaGeS5–] layers separated from one another by alkali metal cations (A+). Each layer is made up of tantalum centered sulfur octahedra and pairs of edge‐sharing germanium centered sulfur tetrahedra. The classical charge valence of these compounds should be represented by [A+][(Ta5+)(Ge4+)(S2–)5]. UV/Vis diffuse reflectance measurements indicate that they are semiconductors with optical bandgaps of ca. 2.0 eV. 相似文献
7.
Dr. Eberhardt Herdtweck Tobias Kornprobst Roland Sieber Leo Straver Johann Plank 《无机化学与普通化学杂志》2011,637(6):655-659
From hydrothermal synthesis needle‐shaped crystals of [Ca3(C6H5O7)2(H2O)2] · 2H2O were obtained. The crystal structure was determined by single‐crystal X‐ray experiments and confirmed by powder data (P$\bar{1}$ (no. 2) a = 5.9466(4), b = 10.2247(8), c = 16.6496(13) Å, α = 72.213(7)°, β = 79.718(7)°, γ = 89.791(6)°, V = 947.06(13) Å3, Z = 2, R1 = 0.0426, wR2 = 0.1037). The structure was obtained from pseudo merohedrically polysynthetic twinned crystals using a combined data collection approach and refinement processes. The observed three‐dimensional network is dominated by eightfold coordinated Ca2+ cations linked by citrate anions and hydrogen bonds between two non‐coordinating crystal water molecules and two coordinating water molecules. 相似文献
8.
Wan‐Feng Lin Qiu‐Ju Xing Jun Ma Jian‐Ping Zou Si‐Liang Lei Xu‐Biao Luo Guo‐Cong Guo 《无机化学与普通化学杂志》2013,639(1):31-34
The new spiroffite Mg2Te3O8 ( 1 ) was prepared by hydrothemal methods and structurally characterized by single‐crystal X‐ray diffraction analysis. Compound 1 crystallizes in the space group C2/c of the monoclinic system with two formula units in a cell: a = 12.6030(7), b = 5.2254(3), c = 11.6331(7) Å, β = 98.6960(10)°, V = 757.30(8) Å3. The structure features a 3D open‐framework with spiroffite topology that has large tunnels approximately 3.2 × 5.5 Å. The optical properties and thermal stability of 1 were characterized by UV and IR spectroscopy as well as TG. Calculations of the electronic band structure along with the density of states (DOS) indicate that the present compound is a semiconductor with an indirect band gap, and that the optical absorption is mainly originated from the charge transitions from O‐2p state to Te‐5p and Te‐5s states. 相似文献
9.
Meng‐Yuan Li Dr. Mohamedally Kurmoo Prof. Zhe‐Ming Wang Prof. Song Gao 《化学:亚洲杂志》2011,6(11):3084-3096
We report the synthesis, crystal structures, thermal and magnetic characterizations of a family of metal‐organic frameworks adopting the niccolite (NiAs) structure, [dmenH22+][M2(HCOO)62−] (dmen=N,N′‐dimethylethylenediamine; M=divalent Mn, 1Mn ; Fe, 2Fe ; Co, 3Co ; Ni, 4Ni ; Cu, 5Cu ; and Zn, 6Zn ). The compounds could be synthesized by either a diffusion method or directly mixing reactants in methanol or methanol–water mixed solvents. The five members, 1Mn , 2Fe , 3Co , 4Ni , and 6Zn are isostructural and crystallize in the trigonal space group P 1c, while 5Cu crystallizes in C2/c. In the structures, the octahedrally coordinated metal ions are connected by anti–anti formate bridges, thus forming the anionic NiAs‐type frameworks of [M2(HCOO)62−], with dmenH22+ located in the cavities of the frameworks. Owing to the Jahn–Teller effect of the Cu2+ ion, the 3D framework of 5Cu consists of zigzag Cu‐formate chains with Cu OCHO Cu connections through short basal Cu O bonds, further linked by the long axial Cu O bonds. 6Zn exhibits a phase transition probably as a result of the order–disorder transition of the dmenH22+ cation around 300 K, confirmed by differential scanning calorimetry and single crystal X‐ray diffraction patterns under different temperatures. Magnetic investigation reveals that the four magnetic members, 1Mn , 2Fe , 3Co , and 4Ni , display spin‐canted antiferromagnetism, with a Néel temperature of 8.6 K, 19.8 K, 16.4 K, and 33.7 K, respectively. The Mn, Fe, and Ni members show spin‐flop transitions below 50 kOe. 2Fe possesses a large hysteresis loop with a large coercive field of 10.8 kOe. The Cu member, 5Cu , shows overall antiferromagnetism (both inter‐ and intra‐chains) with low‐dimensional characteristics. 相似文献
10.
Li7MO6 (M = Bi, Ru, Os) have been synthesized by solid state reaction of Li2O with Bi2O3, or MO2 (M = Ru, Os) and characterized using powder X‐ray diffraction, differential scanning calorimetry, magnetic susceptibility (for M = Ru, Os), ionic conductivity and 6Li solid state NMR (for M = Bi) measurements. All three compounds exhibit a temperature induced triclinic – rhombohedral phase transition. Structures of the new low temperature triclinic phases have been refined by the Rietveld method from powder X‐ray data using atomic parameters of Li7TaO6 as a starting model ( Li7BiO6 : triclinic, , a = 5.5071(1), b = 6.0425(1), c = 5.5231(1) Å, α = 116.912(1), β = 120.867(1), γ = 62.234(1)°, V = 133.96(1) Å3, Z = 1, T = 230 K; Li7RuO6 : triclinic, , a = 5.3654(1), b = 5.8584(1), c = 5.3496(1) Å, α = 117.182(1), β = 119.117(1), γ = 62.632(1)°, V = 124.43(1) Å3, Z = 1, T = 295 K; Li7OsO6 : triclinic, , a = 5.3786(1), b = 5.8725(1), c = 5.3591(1) Å, α = 117.193(1), β = 119.277(1), γ = 62.700(1)°, V = 125.15(1) Å3, Z = 1, T = 295 K). Upon cooling, Li7RuO6 and Li7OsO6 undergo a magnetic transition at 12 and 13 K, respectively, from the paramagnetic to the antiferromagnetic state. The higher ionic conductivity of Li7BiO6 at T < 300 °C, as compared to Li7RuO6 and Li7OsO6, can be ascribed to the undergoing of the triclinic – rhombohedral transition at a much lower temperature. At T > 300 °C, the ionic conductivity of all three compounds increases sharply due to the melting of the lithium sublattice; for Li7RuO6 and Li7OsO6 the latter effect is superimposed by the phase transitions to the rhombohedral modifications. 相似文献
11.
The compound Na3MoO4F was synthesized by high temperature solution methods. Single‐crystal X‐ray diffraction analysis reveals that Na3MoO4F crystallizes in the orthorhombic space group Pnma (No. 62) with lattice constants a = 5.588(2) Å, b = 7.515(3) Å, c = 12.876(5) Å, and Z = 4. The crystal structure consists of isolated MoO4 groups and [FNa3]∞ chains, which are connected by Na–O bonds to form a three‐dimensional framework. A detailed structure comparison between Na3MoO4F and NaMoO3F was carried out. IR spectroscopy and bond valence sum analysis of Na3MoO4F indicate that the structure is reasonable. In addition, the electronic structure was investigated by the first‐principles method. 相似文献
12.
Lingyun Dong Xusheng Ge Pengfei Zhang Qian Li Sufang Sun Shigang Shen 《无机化学与普通化学杂志》2019,645(14):944-948
By the application of cation substitution, a new mixed‐alkali metal diphosphate, K2Li2P2O7, was successfully synthesized through high temperature solution method for the first time. The single‐crystal X‐ray structural analysis shows that it crystallizes in the monoclinic space group C2/c (no. 15), with lattice constants a = 9.814(3) Å, b = 5.5163(15) Å, c = 13.538(4) Å, Z = 4, and β = 110.47(2)°. Its open cage‐like ∞3[Li2(P2O7)]2– framework is built up from alternating arrangement of Li2O6 and P2O7 dimers that form eight and twelve‐membered‐ring channels along the [010] direction, and the K atoms are entrapped in the larger twelve‐membered‐ring channels. Detailed structure comparisons in the N4P2O7 (N = mixed alkali metals) family are discussed. In addition, the structural validity was verified through the IR spectrum. Thermal analyses and UV/Vis/NIR diffuse reflectance spectrum are also performed on the reported compound. 相似文献
13.
The crystal structures of the alkali double salts [Mg(H2O)6]XBr3 (X = Rb+, Cs+) were analyzed in dependence on temperature from laboratory and synchrotron X‐ray powder diffraction data. At room temperature, both compounds are isostructural to [Mg(H2O)6](NH4)Br3 (C2/c; Z = 4; a = 9.64128(6) Å, b = 9.86531(5) Å, c = 13.78613(9) Å, β = 90.0875(5)° for [Mg(H2O)6]RbBr3; a = 9.82304(7) Å, b = 9.98043(6) Å, c = 14.0100(1) Å, β = 90.1430(4)° for [Mg(H2O)6]CsBr3). At a temperature of T = 358 K, [Mg(H2O)6]RbBr3 undergoes a reversible phase transition towards a cubic perovskite type of structure with the [Mg(H2O)6]2+ octahedron in the cuboctahedral cavity exhibiting 4‐fold disorder ( ; a = 6.94198(1) Å at T = 458 K). In case of [Mg(H2O)6]CsBr3 the lattice parameters in dependence on temperature show a distinct kink at T = 340 K, but no symmetry breaking phase transition occurs before decomposition starts. The dominant role of hydrogen bonding with respect to the stability of the crystal structures is discussed. 相似文献
14.
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
15.
Carsten L. Schmidt Ulrich Wedig Dr. Robert Dinnebier Prof. Dr. Martin Jansen Prof. Dr. 《化学:亚洲杂志》2008,3(11):1983-1990
The new barium nitridoosmate oxide (Ba6O)(OsN3)2 was prepared by reacting elemental barium and osmium (3:1) in nitrogen at 815–830 °C. The crystal structure of (Ba6O)(OsN3)2 as determined by laboratory powder X‐ray diffraction ( , No 148: a=b=8.112(1) Å, c=17.390(1) Å, V=991.0(1) Å3, Z=3), consists of sheets of trigonal OsN3 units and trigonal‐antiprismatic Ba6O groups, and is structurally related to the “313 nitrides” AE3MN3 (AE=Ca, Sr, Ba, M=V–Co, Ga). Density functional calculations, using a hybrid functional, likewise indicate the existence of oxygen in the Ba6 polyhedra. The oxidation state 4+ of osmium is confirmed, both by the calculations and by XPS measurements. The bonding properties of the OsN35? units are analyzed and compared to the Raman spectrum. The compound is paramagnetic from room temperature down to T=10 K. Between room temperature and 100 K it obeys the Curie–Weiss law (μ=1.68 μB). (Ba6O)(OsN3)2 is semiconducting with a good electronic conductivity at room temperature (8.74×10?2 Ω?1 cm?1). Below 142 K the temperature dependence of the conductivity resembles that of a variable‐range hopping mechanism. 相似文献
16.
Siti Syaida Sirat Imthyaz Ahmed Khan Omar Bin Shawkataly Mohd Mustaqim Rosli 《无机化学与普通化学杂志》2014,640(10):2019-2024
The reaction of Ru3(CO)10(dotpm) ( 1 ) [dotpm = (bis(di‐ortho‐tolylphosphanyl)methane)] and one equivalent of L [L = PPh3, P(C6H4Cl‐p)3 and PPh2(C6H4Br‐p)] in refluxing n‐hexane afforded a series of derivatives [Ru3(CO)9(dotpm)L] ( 2 – 4 ), respectively, in ca. 67–70 % yield. Complexes 2 – 4 were characterized by elemental analysis (CHN), IR, 1H NMR, 13C{1H} NMR and 31P{1H} NMR spectroscopy. The molecular structures of 2 , 3 , and 4 were established by single‐crystal X‐ray diffraction. The bidentate dotpm and monodentate phosphine ligands occupy equatorial positions with respect to the Ru triangle. The effect of substitution resulted in significant differences in the Ru–Ru and Ru–P bond lengths. 相似文献
17.
18.
Synthesis, crystal structure, thermal stability, and electronic band structure of four new metal antimonides AMSb (A = Rb, Cs; M = Zn, Cd) are reported. CsZnSb and RbZnSb crystallize in the hexagonal ZrBeSi structure type, in a P63/mmc space group (no. 194, Z = 2) and unit cell dimensions of a = 4.5588(2)/4.5466(4) Å and c = 11.9246(6)/11.0999(10) Å. CsCdSb and RbCdSb crystallize in the tetragonal PbFCl structure type in a P4/nmm space group (no. 129; Z = 2) and unit cell parameters of a = 4.8884(5)/4.8227(3) Å and c = 8.8897(9)/8.5492(7) Å. All four compounds are air- and water-sensitive and are shown through DSC measurements to decompose between 975 K and 1060 K. Analysis of the calculated electronic band structure shows that the Zn-containing antimonides are topologically trivial narrow bandgap semiconductors, whereas Cd-containing compounds exhibit a band inversion along Γ-Z direction. 相似文献
19.
Stefan Liebig Heinrich Billetter Tim Wallraff Stefanie Busch Stefan Müller Uwe Ruschewitz 《无机化学与普通化学杂志》2016,642(1):66-72
Three alkali metal acetylides, namely KNaC2, KRbC2, and NaRbC2, were synthesized and characterized by means of X‐ray powder diffraction. KNaC2 and KRbC2 crystallize as a variant of the anti‐PbCl2‐type structure (Pnma, Z = 4), whereas NaRbC2 crystallizes as a variant of the anti‐PbFCl‐type structure (Pmmn, Z = 2). Based on a simple systematic approach developed by Sabrowsky et al. for inter‐alkali metal chalcogenides all known inter‐alkali metal acetylides can be classified into two classes: variants of the anti‐PbCl2 type structure and variants of the anti‐PbFCl type structure. Acetylides with Q(ABC2) ≤ 1.45 crystallize in the anti‐PbCl2‐type structure, whereas for Q(ABC2) > 1.45 the anti‐PbFCl‐type structure is found (Q(ABC2) = Vm(A2C2)/Vm(B2C2) with Vm(A2C2) > Vm(B2C2); Vm: molar volume, A, B = alkali metals). 相似文献
20.
A new zinc phosphite with the formula Zn3(tren)(HPO3)3·xH2O (x≈0.5) has been synthesized under hydrothermal conditions and characterized by FTIR, elemental analysis, powder X‐ray diffraction, single‐crystal X‐ray diffraction, thermogravimetric analysis and its fluorescent spectrum. The compound crystallizes in the triclinic system, space group (No.2), a = 10.1188(9) Å, b = 10.4194(9) Å, c = 10.5176(9) Å, α = 60.763(2)°, β = 70.6150(10)°, γ = 80.725(2)°, V = 912.77(14) Å3, Z = 2. The structure consists of double crankshaft chains, which are linked by Zn‐O‐P bonds to form 8‐ and 12‐membered channels along the [100] direction. The claw‐like Zn‐centered complexes of Zn(N4C6H18) as the supported templates, hang into the 12‐MR channels through Zn‐O‐P linkages with framework. 相似文献