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1.
Arno Pfitzner 《无机化学与普通化学杂志》1995,621(4):685-688
The Crystal Structure of Cu3SbSe3 The hitherto unknown crystal structure of Cu3SbSe3 has been determined from single crystals. The compound crystallizes in the orthorhombic system, space group Pnma (No. 62), with a = 7.9865(8), b = 10.6138(9) and c = 6.8372(7) Å, V = 579.6(1) Å3, Z = 4. Most remarkable feature of the structure are groups of three cis-edge-sharing tetrahedra [Cu3Se8] which are interlinked to a threedimensional arrangement by SbSe3-units. In contrast to Cu3SbS3 in the temperature range from ?180 to 25°C no hints for a phase transition could be detected by means of X-ray- and thermoanalytical methods. 相似文献
2.
(LiI)2Li3SbS3 was prepared by solid‐state reaction of stoichiometric amounts of LiI, Li, Sb, and S in the ratio 2 : 3 : 1 : 3. The product is air and moisture sensitive. The crystal structure was determined from single crystals at room temperature. Colourless to pale yellow (LiI)2Li3SbS3 crystallizes in the orthorhombic system, space group Pnnm (no. 58) with a = 10.436(1)Å, b = 13.509(1)Å, c = 7.530(1)Å, V = 1061.6(1)Å3, and Z = 4 (data at 20 °C). The crystal structure of (LiI)2Li3SbS3 is closely related to that of (CuI)2Cu3SbS3 and (AgI)2Ag3SbS3, at least for the positions of I, Sb, and S. Thus, iodine forms an eutactic arrangement which resembles the structure of hexagonal diamond. [SbS3]3— units are embedded in this framework in a way that the sulphur atoms of two adjacent trigonal pyramids form distorted octahedral voids. The lithium ions are tetrahedrally coordinated and fully ordered within the anionic framework. The three‐dimensional connectivities in (LiI)2Li3SbS3 are significantly different from the homologous copper and silver compound due to the bonding necessities of Li and slightly different radii of the monovalent cations. Thus, a novel three‐dimensional network of edge sharing tetrahedra is observed in (LiI)2Li3SbS3. It exhibits strands of eight‐membered rings of edge sharing tetrahedra which are linked by common vertices and cross linked by double tetrahedra. 相似文献
3.
The new compounds K2Au2Ge2S6 ( 1 ), K2Au2Sn2Se6 ( 2 ), and Cs2Au2SnS4 ( 3 ) have been synthesized through direct reaction of the elements with a molten polyalkalithiogermanate(stannate) flux at 650, 550, and 400 °C, respectively. Their crystal structures have been determined by single crystal X-ray diffraction techniques. 1 crystallizes in the monoclinic space group P21/n with a = 10.633(2) Å, b = 11.127(2) Å, c = 11.303(2) Å, β = 115,37(3)°, V = 1208,2(3) Å3 and Z = 4, final R(Rw) = 0.045(0.106). 2 crystallizes in the tetragonal space group P4/mcc with a = 8.251(1) Å, c = 19.961(4) Å, V = 1358,9(4) Å3 and Z = 4, final R(Rw) = 0.040(0.076). 3 crystallizes in the orthorhombic space group Fddd with a = 6.143(1) Å, b = 14.296(3) Å, c = 24.578(5) Å, V = 2158.4(7) Å3 and Z = 4, final R(Rw) = 0.039(0.095). The structures of 1 , 2 , and 3 consist of infinite, one-dimensional anionic chains containing X2Q64– units linked by Au+ ions and charge balancing K+/Cs+ ions situated between the chains. All compounds were investigated with differential thermal analysis, FT-IR, and solid state UV/VIS diffuse reflectance spectroscopy. 相似文献
4.
The two novel thioantimonate(V) compounds [Mn(C6H18N4)(C6H19N4)]SbS4 ( I ) and [Mn(C6H14N2)3][Mn(C6H14N2)2(SbS4)2]·6H2O ( II ) were synthesized under solvothermal conditions by reacting elemental Mn, Sb and S in the stoichiometric ratio in 5 ml tris(2‐aminoethyl)amine (tren) at 140 °C or chxn (trans‐1, 2‐diaminocyclohexane, aqueous solution 50 %) at 130 °C. Compound I crystallises in the triclinic space group P1¯, a = 9.578(2), b = 11.541(2), c = 12.297(2)Å, α = 62.55(1), β = 85.75(1), γ = 89.44(1)°, V = 1202.6(4)Å3, Z = 2, and II in the monoclinic space group C2/c, a = 32.611(2), b = 13.680(1), c = 19.997(1)Å, β = 117.237(5)°, V = 7931.7(8)Å3, Z = 4. In I the Mn2+ cation is surrounded by one tetradentate tren molecule, one protonated tren acting as a monodentate ligand and a monodentate [SbS4]3— anion yielding a distorted octahedral environment. In II one unique Mn2+ ion is in an octahedral environment of three bidentate chxn molecules and the second independent Mn2+ ion is coordinated by two chxn ligands and two monodentate [SbS4]3— units leading to a distorted octahedral surrounding. The compounds were investigated and characterized with thermal and spectroscopic methods. 相似文献
5.
Ehab M. Al‐Shami Adnan S. Abu‐Surrah Martti Klinga Hamdallah A. Hodali 《无机化学与普通化学杂志》2002,628(6):1433-1436
The phosphorus‐sulfur ligand 1‐(methylthio)‐3‐(diphenylphosphino)‐propane (S‐P3) has been synthesized and characterized by 1H NMR and 13C NMR. Reactions of S‐P3 with [PdCl2(PhCN)2] afforded the complexes [PdCl2(S‐P3)] ( I ) and [PdCl2(S‐P3)2] ( II ), in which S‐P3 acts as a bidentate and monodentate ligand, respectively. Compound I crystallizes in monoclinic space group P21/n (No. 14) with cell dimensions: a = 8.589(3), b = 15.051(3), c = 17.100(3)Å, β = 102.91(2)°, V = 2154.7(9)Å3, Z = 4. Likewise, compound II crystallizes in monoclinic space group P21/n (No. 14) with a = 9.993(5), b = 8.613(4), c = 18.721(5)Å, β = 90.18(3)°, V = 1611.3(12)Å3, Z = 2. Compound II has a trans square planar configuration with only the P‐site of the ligand bonded to the palladium atom. 相似文献
6.
Synthesis, Structure, and Reactions of Vanadium Acid Esters VO(OR)3: Transesterification and Reaction with Oxalic Acid The reaction of tert.‐Butyl Vanadate VO(O‐tert.Bu)3 ( 1 ) with H2C2O4 in the primary alcohols ethanol and propanol results in the formation of (ROH)(RO)2OVV(C2O4)VVO(OR)2(HOR) (with R = C2H5 2 and R = C3H7 3 ). Compounds 2 and 3 are the first structurally characterized neutral, binuclear oxo‐oxalato‐complexes with pentavalent vanadium. The two vanadium atoms are connected by a bisbidentate oxalate group. The {VO6} coordination at each vanadium site is completed by a terminal oxo group, an alcohol ligand and two alcoxide groups. The binuclear molecules are connected to chains by hydrogen bonding. In the case of 2 a reversible isomorphic phase transition in the temperature range of –90 °C to –130 °C is observed. From methanolic solution the polymeric Methyl Vanadate [VO(OMe)3] ( 4 ) was obtained by transesterification. A report on the crystal structures of 1 , 2 and 3 as well as a redetermination of the structure of 4 is given. Crystal data: 1, orthorhombic, Cmc21, a = 16.61(2) Å, b = 9.274(6) Å, c = 10.784(7) Å, V = 1662(2) Å3, Z = 4, dc = 1.144 gcm–1; 2 (–90 ° C) , monoclinic, I2/a, a = 33.502(4) Å, b = 7.193(1) Å, c = 15.903(2) Å und β = 143.060(3)°, V = 2303(1) Å3, Z = 4, dc = 1.425 gcm–1; 2 (–130 ° C) , monoclinic, I2/a, a = 33.274(4) Å, b = 7.161(1) Å, c = 47.554(5) Å, β = 142.798(2)°, V = 6851(1) Å3, Z = 12, dc = 1.438 gcm–1; 3 , triklinic, P1, a = 9.017(5) Å, b = 9.754(5) Å, c = 16.359(9) Å, α = 94.87(2)°, β = 93.34(2)°, γ = 90.42(2)°, V = 1431(1) Å3, Z = 2, dc = 1.340 gcm–1; 4 , triklinic, P1, a = 8.443(2) Å, b = 8.545(2) Å, c = 9.665(2) Å, α = 103.202(5)°, β = 96.476(5)°, γ = 112.730(4)°, V = 610.2(2)Å3, Z = 4, dc = 1.742 gcm–1. 相似文献
7.
Tetraphenylphosphonium 5‐nitrotetrazolate ( 2 ) was prepared by metathesis of sodium 5‐nitrotetrazolate dihydrate ( 1 ; NaNT) with tetraphenylphosphonium chloride in acetone. The new compound was fully characterized by vibrational (IR, Raman) and NMR (1H, 13C, and 14N) spectroscopies, elemental analysis, and mass spectrometry. Attempted synthesis of 2‐methyl‐5‐nitrotetrazole (2‐MeNT) by methylation of 1 with dimethylsulfate at reflux from acetonitrile failed, and crystals of an explosive compound with the formula (NaNT)2(H2O)2CH3CN ( 3 ), NT = 5‐nitrotetrazolate, formed. X‐ray diffraction techniques were used to determine the crystal structure of 2 and 3 . Compound 2 crystallizes in the orthorhombic space group P212121 with four molecules in the unit cell and unit cell parameters a = 7.7413(4) Å, b = 13.624(1) Å, c = 21.252(1) Å, and V = 2241.5(2) Å3, whereas 3 crystallizes in the orthorhombic space group Ama2 with four formula unit in the unit cell and unit cell parameters a = 14.805(6) Å, b = 9.908(4) Å, c = 8.940(3) Å, and V = 1311.4(1) Å3. © 2009 Wiley Periodicals, Inc. Heteroatom Chem 20:35–44, 2009; Published online in Wiley InterScience ( www.interscience.wiley.com ). DOI 10.1002/hc.20509 相似文献
8.
Michael Schaefer Ralph Sthler Wolff‐Ragnar Kiebach Christian Nther Wolfgang Bensch 《无机化学与普通化学杂志》2004,630(12):1816-1822
Four new thioantimonate(III) compounds with the general formula [TM(tren)]Sb4S7, TM = Mn 1 , Fe 2 , Co 3 and Zn 4 , were synthesized under solvothermal conditions by reacting elemental TM, Sb and S in an aqueous solution of tren (tren = tris(2‐aminoethyl)amine). All compounds crystallize in the monoclinic space group P21/n with four formula units in the unit cell. Single crystal X‐ray analyses of 1 [a = 8.008(2), b = 10.626(2), c = 25.991(5) Å, β = 90.71(3)°, V = 2211.4(8) Å3], 2 [a = 8.0030(2), b = 10.5619(2), c = 25.955(5) Å, β = 90.809(3)°, V = 2193.69(8) Å3], 3 [a = 7.962(2), b = 10.541(2), c = 25.897(5) Å, β = 90.90(3)°, V = 2173.0(8) Å3] and 4 [a = 7.978(2), b = 10.625(2), c = 25.901(5) Å, β = 90.75(3)°, V = 2195.2(8) Å3] reveal that the compounds are isostructural. The [Sb4S7]2‐ anions are composed of three SbS3 trigonal pyramids and one SbS4 unit as primary building units (PBU). The PBUs share common edges and corners to form semicubes (Sb3S4) which may be regarded as secondary building units (SBU). The SBUs and SbS3 pyramids are joined in an alternating fashion yielding the equation/tex2gif-stack-1.gif[Sb4S7‐] anionic chain which is directed along [100]. Weaker Sb‐S bonding interactions between neighbored chains lead to the formation of layers within the (001) plane which contain pockets that are occupied by the cations. The TM2+ ions are in a trigonal bipyramidal environment of four N atoms of the tren ligand and one S atom of the thioantimonate(III) anion. The optical band gaps depend on the TM2+ ion and amount to 3.11 eV for 1 , 2.04 eV for 2 , 2.45 eV for 3 , and 2.60 eV for 4 . 相似文献
9.
Michal W. Wieczorek Wieslaw Majzner Magdalena Sikora Jzef Kula 《Heteroatom Chemistry》1995,6(6):525-531
During the transformation process of limonene to tetrahydrofuran derivatives, the title compounds (±)-( 4 ) have been obtained as crystalline products and subjected to X-ray analysis. The crystals of trans-( 4 ) are orthorhombic, space group P212121, with the lattice constants a = 7.0445(5) Å, b = 10.0908(4) Å, c = 14.0309(6) Å; the absolute configuration at atoms C1, C2, and C4 is Rc1, Sc2, and Rc4, respectively. The isomeric form cis-( 4 ) crystallizes in the monoclinic system, space group P21, with the following unit-cell parameters: a = 10.8275(4) Å, b = 8.6994(5) Å, c = 16.4722(6) Å, β = 106.515(3)°. The asymmetric part of the unit cell of cis-( 4 ) contains three independent molecules. Each of these three molecules has the identical absolute configuration at all centers of chirality: Sc1, Sc2, and Rc4. © John Wiley & Sons, Inc. 相似文献
10.
Guo-Quing Wu Zhongjia Tang Yongxian Yu Pingdi Lin M. Jansen K. Knigstein 《无机化学与普通化学杂志》1992,610(4):135-138
Phosphates MEuPO4 with M = K, Rb, and Cs were synthesized by the reduction of EuPO4 with alkali metal vapour under 1 Pa of argon pressure at 260–530°C in sealed tantalum or niobium lined glass tubes. All the compounds belong to the β-K2SO4 orthorhombic structure with a = 7.359(3), b = 9.630(4), c = 5.569(2) Å, V = 394.7(2) Å3 for KEuPO4, a = 7.462(3), b = 9.797(3), c = 5.649(2) Å, V = 413.0(2) Å3 for RbEuPO4 and a = 7.889(2), b = 10.099(2), c = 5.820(4) Å, V = 463.6(2) Å3 for CsEuPO4. Samples are stable and not hygroscopic in air at room temperature but hydrolyse to Eu5(PO4)3OH, hexagonal, a = 9.764(2), c = 7.262(2) Å, on heating in water and decompose to Eu3(PO4)2, hexagonal, a = 5.393(1), c = 19.838(3) Å, under argon at ca. 600°C. All the five compounds are paramagnetic. 相似文献
11.
By means of alternating current electrochemical synthesis crystals of [C13H15N2]+2[CuCl2.58Br1.42]– ( I ) and [C13H15N2]+[Cu2Cl0.67Br2.33]– ( II ) have been obtained and structurally characterized. Compound I crystallizes in the orthorhombic system, space group Fddd, a = 7.828(1) Å, b = 26.402(2) Å, c = 28.595(3) Å, Dc = 1.4995(5) g/cm3, Z = 8, R = 0.067 for 2157 reflections. The CuX42– tetrahedra are connected with the organic cations through an electrostatic interaction. Crystals of II are monoclinic, space group P21/c, a = 9.2293(8) Å, b = 22.1332(9) Å, c = 9.2939(9) Å, β = 118.021(4)°, Dc = 2.1251(5) g/cm3, Z = 4, R = 0.042 for 2858 reflections. A tetrahedral environment of the Cu1 atom involves four halide atoms, whereas Cu2 possesses a trigonal‐pyramidal coordination with the C=C‐bond and three halide atoms. 相似文献
12.
A new diiron complex has been synthesized and characterized by X‐ray single crystal structural analysis: [FeII(phen)3][FeIII2OCl6]·2CH3CN. The complex crystallizes in the monoclinic system, space group C2/c, with lattice parameters a = 21.162(4) Å, b = 15.168(3) Å, c = 14.812(3) Å, β= 112.71 (3)°, V = 4385.8(15) Å3, Dx = 1.543 Mg/m3, Z = 4. The corresponding variable temperature susceptibility measurement shows that there exists an antiferromagnetic interaction in the complex. 相似文献
13.
The reaction of (S)-(-)-1, l-diphenyl-propane-1,2-diol with AlCl3 in diethyl ether furnishes the product [Al((S)-(-)-μ2-OC(H)(Me)C(Ph)2OH)Cl2]2 1, which decomposes slowly above 25 °C. Complex 1·2Et2O Crystallizes in the non-centrosymmetric monoclinic space group P21 with a=10.591(1) Å, b=16.718(1) Å, c = 12.156(2) Å, β=99.30(2)°, V = 2124.1(3) Å3, z = 4, R = 4.67%, Rw=4.84%, GoF=1.14. The structure of 1 shows a dimer feature, which is hydrogen bonded to two diethyl ether molecules. In the reaction of 2-phenoxyethanol with AlMe3, the dimeric [(μ-O(CH2)2OPh)AlMe2]2 is obtained in high yield. 2 crystallizes in the monoclinic space group P21/c with a = 7.398(2) Å, b = 7.376(2) Å, c = 20.710(2) Å, β = 90.56(2)°, v = 1129.9(4) Å3, z=4, R=5.70%, Rw=7.15%, GoF=1.59. 相似文献
14.
The new phosphides HfM′P (M′ = Fe, Co, Ni) have been synthesized by arc melting of HfP and the corresponding 3 d metal, and subsequent annealing at 1400°C. The lattice constants vary from a = 6.247(2) Å, b = 3.7177(6) Å, c = 7.137(2) Å, V = 165.74(8) Å3 for HfFeP, a = 6.295(3) Å, b = 3.668(2) Å, c = 7.175(4) Å, V = 165.7(2) Å3 for HfCoP to a = 6.240(3) Å, b = 3.716(2) Å, c = 7.135(2) Å, V = 165.4(2) Å3 (HfNiP) in the orthorhombic space group Pnma. Although ZrNiP occurs only in the Ni2In structure type, all three Hf phosphides crystallize in the Co2Si structure type, isotypic to ZrFeP and ZrCoP. The structural differences between HfNiP and ZrNiP can be explained by the preference of Hf for structures with more metal-metal bonds rather than by size effects. 相似文献
15.
The reaction of K2S5, Cu, Gd, and S in a 2 : 1 : 2 : 4 molar ratio at 450 °C yields yellow-orange needle-like cuboids of the new quaternary compound KCuGd2S4. The crystal structure represents a novel three-dimensional structure type of quaternary rare earth chalcogenides with alkali metal. The compound crystallizes in the orthorhombic space group Cmcm (No. 63) with a = 3.9921(1) Å, b = 13.523(3) Å, c = 13.802(3) Å, V = 745.1(3) Å3, Z = 4. In the structure GdS6 octahedra and CuS4 tetrahedra are joined by common edges and corners forming corrugated layers parallel to (010). The GdS6 octahedra are connected via common edges in the third dimension thus leading to the formation of a three-dimensional tunnel structure. The potassium cations are confined within the pentagonal shaped channels and are surrounded by eight sulfide anions each. 相似文献
16.
Steffen Pütz Matthias Döch Arno Lindemann Adrienne Hammerschmidt Bernt Krebs 《Phosphorus, sulfur, and silicon and the related elements》2013,188(4-5):937-939
We now report the synthesis and crystal structure of LiBSe3, a new perselenoborate with anionic layers. LiBSe3 crystallizes in the orthorhombic space group Pca21 (No. 29), a = 12.770(3) Å, b = 5.777(2) Å, c = 10.726(2) Å. 相似文献
17.
The reaction of 2‐amino‐benzothiazole with allyl bromide resulted in a mixture of 2‐imino‐3‐allyl‐benzothiazole and 2‐imino‐3‐allyl‐benzothiazolium bromide.Using such a mixture and copper(II) chloride in acetonitrile solution in alternating‐current electrochemical synthesis crystals of the [(CuCl)C10H10SN2] ( I ) have been obtained. The same procedure, performed in ethanol solution, has led to formation of [C10H11SN2+]2[Cu2Cl4]2? ( II ). In the same manner the bromine derivative [C10H11SN2+]2[Cu2Br4]2? ( III ) has been synthesized. All three compounds were X‐ray structurally investigated. I :monoclinic space group P21/n, a = 13.789(6), b = 6.297(3), c = 13.830(6) Å, β = 112.975(4)°, V = 1105.6 (9) Å3, Z = 4 for CuCl·C10H10 SN2 composition. Compounds II and III are isomorphous and crystallize in triclinic space group. II a = 7.377(3), b = 8.506(3), c = 9.998(4) Å, α = 79.892(10)°, β = 82.704(13)°, γ = 78.206(12)°, V = 601.9(4) Å3, Z = 1. III a = 7.329(2), b = 8.766(3), c = 10.265(3) Å, α = 79.253(9)°, β = 82.625(9)°, γ = 77.963(9)°, V = 630.9(3) Å3, Z = 1. In the structure I [(CuCl)C10H10SN2] building blocks are bound into infinitive spiral‐like chains via strong N‐H..Cl hydrogen bonds. In the zwitter‐ionic II and III compounds copper and halide atoms form centrosymmetric [Cu2X4]2? anions, which are interconnected via N‐H..X hydrogen bonds into infinite butterfly‐like chains. The strongest Cu‐(C=C) π‐interaction has been observed in structure I , where copper possesses coordination number 3. Increasing copper coordination number to 4 in II as well as replacing chlorine atoms by bromine ones in III suppresses markedly this interaction. 相似文献
18.
Karina Möller Christian Näther Alexander Bannwarth Wolfgang Bensch Prof. Dr. 《无机化学与普通化学杂志》2007,633(15):2635-2640
The new charge neutral complex [Cr(tren)SbS3]·H2O was synthesized under solvothermal conditions applying CrCl3·6H2O, Sb2S3, and S as starting material in an aqueous tren solution (tren = tris(2‐aminoethyl)amine)). The compound crystallizes in the non‐centrosymmetric space group P212121 with a = 8.7779(15), b = 10.7122(17), c = 15.4286(18) Å, V = 1450.8(4) Å3. In the structure the Cr3+ ion is surrounded by four N atoms of the amine molecules and by two S atoms of a trigonal pyramidal [SbS3]3? group, i.e., the latter acts as a bidentate ligand. A three‐dimensional network is formed via hydrogen bonds between the complexes and water molecules. The main resonances in the Raman spectrum can be explained on the basis of calculated data. The most intense band is due to the Sb‐S stretching vibration. The thermal properties were investigated by DTA‐TG measurements. On heating [Cr(tren)SbS3]·H2O decomposes in two distinct steps. The first step corresponds to the removal of the water molecules and the second step to the loss of the tren ligand. 相似文献
19.
1. The system Li? Cu? P was investigated by phase analysis. The samples were prepared at 500–600°C. The resulting ternary phases were characterized mainly by x-ray investigation. 2. At 560°C the range of homogeneity of Cu 3 P lies between 25.6–26.7 atomic % P. Cu3P forms a high-temperature (HT) modifikation, which crystallizes in a hexagonal subcell of the low-temperature (TT) modification (Z = 6): a = 4.09, c = 7.19 Å, c/a = 1.76; Z = 2 at 560°C. The intensities of the HT-powder pattern could be explained by a model in the space group P3 ml—D33d, which was deduced from TT-Cu3P. 3. Li 2 CuP , which can be derived from Li3P, crystallizes hexagonally with a = 16.18, c = 7.724 Å; c/a = 0.477; Z = 32. In the structure, copper occupies the Li position with lowest number and coordination. 4. LiCu 2 P also crystallizes hexagonally with a = 12.08, c = 7.39 Å; c/a = 0.71; Z = 18. In the direction [001] there is a disordered superlattice. The lattice constants of the high-temperature modification of LiCu2P, which are related to those of HT-Cu3P, at 520°C are: a = 4.08, c = 7.44 Å; c/a = 1.82; Z = 2. The interpretation of the intensities of the powder patterns did not result in a plain model related to HT-Cu3P when calculated for the space group P3 m1—D33d. 5. LiCu 2 P 2 crystallizes tetragonally with a = 3.887, c = 9.554 Å; c/a = 2.46; Z = 2. The structure determination gave the D13-type lattice. The space group is No. 139 I4/mmm—D174h, the atoms occupy the following positions: 2 Li in (2a), 4 Cu in (4d) and 4 P in (4e) with z = 0.388. The compound shows P2 groups parallel to [001] with a P? P distance of 2.14 Å. 6. Li 1,75 Cu 1,25 P 2 crystallizes orthorhombically with a = 3.874, b = 12.668, c = 8.743 Å; Z = 6. The crystal structure has been determined. The atoms occupy the following positions within the space group No. 71 Immm—D152h: 2 Li in (2a), 4 Li in (4g) with y = 0.27, 4 Li in (4j) with z = 0.33, 7.5 Cu in (8l) with y = 0.127 and z = 0.267, 8 P in (8l) with y = 0.352 and z = 0.377, and 4 P in (4h) with y = 0.085. This structure, too, is dominated by the occurence of P2 groups, which are oriented as well parallel [001] as parallel [010]. 相似文献
20.
Synthesis and Structure of New Sodium Hydrogen Sulfates Na(H3O)(HSO4)2, Na2(HSO4)2(H2SO4), and Na(HSO4)(H2SO4)2 Three acidic sodium sulfates have been synthesized from the system sodium sulfate/sulfuric acid and have been crystallographically characterized. Na(H3O)(HSO4)2 ( A ) crystallizes in the space group P21/c with the unit cell parameters a = 6.974(2), b = 13.086(2), c = 8.080(3) Å, α = 105.90(4)°, V = 709.1 Å3, Z = 4. Na2(HSO4)2(H2SO4) ( B ) is orthorhombic (space group Pna21) with the unit cell parameters a = 9.970(2), b = 6.951(1), c = 13.949(3) Å, V = 966.7 Å3 and Z = 4. Na(HSO4)(H2SO4)2 ( C ) crystallizes in the triclinic space group P1 with the unit cell parameters a = 5.084(1), b = 8.746(1), c = 11.765(3) Å, α = 68.86(2)°, β = 88.44(2)°, γ = 88.97(2)°, V = 487.8 Å3 and Z = 2. All three compounds contain SO4 tetrahedra as HSO4? anions and additionally in B and C in form of H2SO4 molecules. The ratio H:SO4 determines the connectivity degree in the hydrogen bond system. In A , there are zigzag chains and dimers additionally connected via oxonium ions. Complex chains consisting of cyclic trimers (two HSO4? and one H2SO4) are present in B . In structure C , several parallel chains are connected to columns due to the greater content of H2SO4. Sodium cations show a distorted octahedral coordination by oxygen in all three structures, the NaO6 octahedra being “isolated” (connected via SO4 tetrahedra only) in A . Pairs of octahedra with common edge form Na2O10 dimeric units in C . Such double octahedra are connected via common corners forming zigzag chains in B . 相似文献