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1.
Abbas Taeb Harald Krischner Christoph Kratky 《Monatshefte für Chemie / Chemical Monthly》1987,118(6-7):727-731
Sr(N3)2 · OC(NH2)2 was prepared by the reaction of Sr(N3)2 with urea in aqueous solution. The crystals are monoclinic,a=12.993 (4),b=7.177 (1),c=7.896 (1) Å, =98.98 (1)°, space group P 21/a,N=4. The crystal structure was determined by single crystal X-ray methods and refined toR
w=0.086. The crystal structure consists of [SrN6O2]-antiprism which are linked to form layers parallel 001. 相似文献
2.
Synthesis and Crystal Structure of the First Oxonitridoborate — Sr3[B3O3N3] The cyclotri(oxonitridoborate) Sr3[B3O3N3] was synthesized at 1450 °C as coarsely crystalline colourless crystals by the reaction of SrCO3 with poly(boron amide imide) using a radiofrequency furnace. The structure was solved by single‐crystal X‐ray diffractometry (Sr3[B3O3N3], Z = 4, P21/n, a = 663.16(2), b = 786.06(2), c = 1175.90(3) pm, η = 92.393(1)°, R1= 0.0441, wR2 = 0.1075, 1081 independent reflections, 110 refined parameters). Besides Sr2+ there are hitherto unknown cyclic [B3O3N3]6— ions (B—N 143.7(10) — 149.1(9) pm, B—O 140.5(8) — 141.4(8) pm). 相似文献
3.
Volodymyr Smetana Volodymyr Babizhetskyy Grigori V. Vajenine Arndt Simon Prof. Dr. Dr.h.c. 《无机化学与普通化学杂志》2008,634(5):849-852
Preparation and Crystal Structures of Li26Na58Ba38Ex Phases (E = N, H; x = 0 – 1) Li26Na58Ba38Ex (E = N, H; x = 0–1) were prepared as a majority phase by the reactions of the metals with Ba(N3)2 or BaH2 at 250 °C for five days. According to single crystal and powder X‐ray diffraction investigation, all compounds are cubic, space group with the unit cell parameter a ranging from 27.335(2) (x = 0) to 27.554(3) (x = 1, E = N, H) Å and Z = 4. This compound series can be described as a filled variant of Li13Na29Ba19, in which nitrogen or hydrogen atoms are found in the centre of Li26 clusters in tetrahedral environment. Li26Na58Ba38Ex represents a new group of metal‐rich compounds extending the growing family of subnitrides. 相似文献
4.
Franz Andreas Mautner Harald Krischner Christoph Kratky 《Monatshefte für Chemie / Chemical Monthly》1988,119(11):1245-1249
[N(CH3)4]Ca(N3)3,M=240.29, was prepared from aqueous solutions of tetramethylammoniumazide with calciumazide at 298 K. The crystals are tetragonala=936.6(7) pm,c=694.7(5)pm, space group P4/nmm,Z=2, (x)=1.31Mgm–3. The crystal structure was determined by single crystal x-ray diffraction (234 Mo-K-reflections, =0.469 mm–1,R=0.064). Calcium is octahedrally coordinated to six azide groups. The octahedra are connected via azide groups to a threedimensional array with the complex ammonium ions between. The terminal nitrogen atoms of the azide groups and the methyl groups are considerably disordered. 相似文献
5.
Preparation and Crystal Structure of Diammin Magnesium Diazide Mg(NH3)2(N3)2 Diammin magnesium diazide was synthesized from Mg3N2 and NH4N3 in liquid ammonia and crystallized at 150 °C under autogenous atmosphere of HN3 and NH3 using sealed ampoules. Mg(NH3)2(N3)2 is a colorless, microcrystalline powder which can detonate above 180 °C. Caution, preparation and manipulation of Mg(NH3)2(N3)2 is very dangerous! The crystal structure was solved from powder data using the Patterson method and a Rietveld refinement was performed (Mg(NH3)2(N3)2, I 4/m, no. 87; a = 6.3519(1), c = 7.9176(2) Å; Z = 2, R(F2)= 0.1162). The crystal structure of Mg(NH3)2(N3)2 is related to that of SnF4. It consists of planes built up from corner sharing Mg(NH3)2(N3)4 octahedra connected equatorially over their four azide bridges with the ammonia ligands being in trans position. IR data were collected and interpreted in accordance with the structural data. 相似文献
6.
Synthesis and Crystal Structure of the Ionic Tellurium Nitride Chloride[Te3N2Cl5(SbCl5)]+SbCl6? The title compound has been prepared by the reaction of Te2NCl5 with antimony pentachloride in CH2Cl2 suspension. It is characterized by IR spectroscopy and by a crystal structure determination. Space group P21/c, Z = 4, lattice dimensions at ?70°C: a = 1535.6, b = 1259.5, c = 1572.4 pm, β = 109.30°, R = 0.031. The compound forms an ionic pair with the central group of a (TeNCl)2 molecule in which the tellurium atoms are linked by the nitrogen atoms to give a planar Te2N2 four-membered ring. One of the nitrogen atoms is coordinated by a TeCl3+ unit, the other one by an antimony pentachloride molecule. According to the IR spectra a structure like [Te2N2Cl2(TeCl4)2] is proposed for Te2NCl5. 相似文献
7.
Beatrice Kern Hannes Vitze Michael Bolte Matthias Wagner Hans‐Wolfram Lerner 《无机化学与普通化学杂志》2008,634(11):1830-1832
The lithium silanolate LiOSiMe3 is accessible from the reaction of Me3SiOSiMe3 with LiMe in tetrahydrofuran. Single crystals of [Li7(OSiMe3)7(THF)] were obtained from toluene at 25 °C. The structure of [Li7(OSiMe3)7(THF)] (C2/c) features a capped trigonal antiprismatic arrangement of seven Li atoms. The Li atoms in [Li7(OSiMe3)7(THF)] are μ3‐bridged by seven O atoms of the silanolate ligand. 相似文献
8.
Synthesis and Crystal Structure of Sr2Rh7P6 Single crystals of Sr2Rh7P6 were obtained by reaction of the elements in molten lead at 1100 °C and investigated by X-ray methods. The compound crystallizes tetragonally (a = 11.080(2), c = 4.098(1) Å) and forms a crystal structure (P 4 21m; Z = 2) with ThCr2Si2 analogous units, which are linked with each other in a new way. Therefore the RhP4 tetrahedra form bands of edge sharing chains parallel to [001] anstead of layers as in the ThCr2Si2 type structure. The arrangement enables a part of the P atoms to form short P–P distances of 2,26 Å and space for additional Rh atoms with a likewise distorted tetrahedral coordination of P atoms is obtained. 相似文献
9.
Lithium and Cesium Alkoxometalates The aluminium alkoxide, Al(OCH2Ph)3 ( 1 ), can be obtained from a direct synthesis of Al and PhCH2OH under HgCl2 catalysis. The formation of the metalate [{(Diglyme)Li}{Al(OtBu)4}] ( 2 ) from LiAlH4 and tBuOH in THF under evolution of hydrogen takes place, if the reaction product is heated under reflux with additional tBuOH in diglyme. The nucleophilic attack of F– ions leads during the treatment of CsF on a THF solution of Al(OcHex)3 after ligand redistribution to the coordination polymer [{Cs(THF)2}{Cs(THF)}{Al(OcHex)4}2]n ([3]n). 1 , 2 , and 3 were characterized by NMR, IR and MS techniques as well as by crystal structure analyses. According to them 1 is present as tetramer in solution and the solid state. The central structural motif of the metalate 2 is a heteronuclear and planar LiO2Al four‐membered ring with a penta‐coordinated Li+ ion. In the chainlike coordination polymer [ 3 ]n Cs+ ions with coordination number five and six occupy alternating positions. 相似文献
10.
Syntheses and Crystal Structures of the Rhenium(VII) Nitride Chlorides ReNCl4 and ReNCl4·H2O Rhenium(VII) nitride chloride, ReNCl4 ( 1 ) is obtained in form of brown needles with metallic luster by the reaction of ReCl5 with Cl3VNCl at 140 °C under vacuum in a sealed glass ampoule. It crystallizes in the tetragonal space group I4 with the lattice parameters a = 826.7(4), c = 405.1(2) pm, and Z = 2. The square pyramidal molecules are connected by asymmetric nitrido bridges to form chains along the crystallographic c axis. The shorter Re‐N distance of 163.0(5) pm corresponds to a triple bond, while the pronounced longer distance of 242.0(5) pm can be interpreted with a weak donor bond. The reaction of ReCl5 with VN at 170 °C under vacuum in a sealed glass ampoule yields red needles of ReNCl4·H2O ( 2 ). It crystallizes in the orthorhombic space group Pnma with a = 1075.4(2), b = 1108.5(2), c = 547.7(5) pm and Z = 4. The Re atoms exhibit a distorted octahedral coordination with the aqua ligand in trans position to the nitrido ligand. The Re‐N triple bond has a bond distance of 166.1(11) pm. The complexes are connected by hydrogen bridges O‐H···N to form chains. 相似文献
11.
12.
Synthesis and Crystal Structure of the known Zintl Phases Cs3Sb7 and Cs4Sb2 Cs3Sb7 and Cs4Sb2 were synthesized from the elements and their crystal structures were determined on the basis of single crystal x‐ray data. Cs3Sb7 crystallizes in the monoclinic system with space group P21/c (a = 1605.7(1) pm, b = 1571.1(1) pm, c = 2793.9(2) pm, β = 96.300(2)°, Z = 16) and contains anions Sb73–. In the structure of Cs4Sb2 (orthorhombic, space group Pnma, a = 1598.5(3) pm, b = 631.9(2) pm, c = 1099.5(2) pm, Z = 4) dumbbells Sb24– are present. 相似文献
13.
14.
Synthesis and Crystal Structure of the Tellurium Nitride Chloride [Te11N6Cl26] The title compound has been prepared by the reaction of tellurium tetrachloride with tris(trimethylsilyl)amine in boiling toluene. Pale yellow crystals of the composition [Te11N6Cl26]2 · 9C7H8 are obtained by cooling of the saturated solution. The compound was characterized by IR spectroscopy and by a crystal structure determination. Space group P1 , Z = 1, structure solution with 5912 observed unique reflections, R = 0.043. Lattice dimensions at ?50°C: a = 1636.2, b = 1692.7, c = 1704.1 pm, α = 60.57°, β = 69.59°, γ = 64.29°. The dominating structural element of the nitrchloride are planar Te5N3 units forming two four-member Te2N2 rings which are condensed together. Two asymmetric units [Te11N6Cl26] are linked by a centre of symmetry; the intercalated toluene molecules are without binding interactions. 相似文献
15.
The Crystal Structure of cis‐ and trans‐N‐iso‐Propylamidodimethyl Indium, [(CH3)2In‐N(H)iC3H7]2 According to the X‐ray structure determination [(CH3)2In‐N(H)iC3H7]2 (prepared from InMe3 (Me = CH3) and H2NiPr (iPr = CH(CH3)2) crystallizes in the monoclinic space group P21/n with 3 dimeric trans as well as 3 dimeric cis isomers per unit cell. The centrosymmetric form has a planar In2N2 core with In—N bonds of 222.1(4) and 222.9(5) pm, respectively, the skeleton of the cis isomer with In—N bonds of 221.4(4) pm is slightly folded (13.7°). Some 1H, 13C NMR, IR, and Raman data are reported. 相似文献
16.
Preparation and Crystal Structure of Tetramethylammoniumbromide‐Bromine‐Sulfur Dioxide Adduct, [(CH3)4N]+Br‐�Br2�2SO2 Tetramethylammoniumtribromide forms with sulfur dioxide a salt which is characterized by vibrational spectroscopy and crystal structure analysis. [(CH3)4N]+Br‐�Br2�2SO2 crystallizes monoclinic in the space group P21/m with a = 657.4(5) pm, b = 2933.0(5) pm, c = 1462.2(5) pm, β = 91.241(5)° and four formula units in the unit cell. The crystal structure possesses bent infinite chains which consist of alternately arranged bromine and bromide ions. The bromide ions are connected to the molecules of bromine and sulfur dioxide by strong interactions forming a three dimensional network. 相似文献
17.
Investigations on the Crystal Structure of Lithium Dodecahydro‐closo‐dodecaborate from Aqueous Solution: Li2(H2O)7[B12H12] By neutralization of an aqueous solution of the acid (H3O)2[B12H12] with lithium hydroxide (LiOH) and subsequent isothermic evaporation of the resulting solution to dryness, it was possible to obtain the heptahydrate of lithium dodecahydro‐closo‐dodecaborate Li2[B12H12] · 7 H2O (≡ Li2(H2O)7[B12H12]). Its structure has been determined from X‐ray single crystal data at room temperature. The compound crystallizes as colourless, lath‐shaped, deliquescent crystals in the orthorhombic space group Cmcm with the lattice constants a = 1215.18(7), b = 934.31(5), c = 1444.03(9) pm and four formula units in the unit cell. The crystal structure of Li2(H2O)7[B12H12] can not be described as a simple AB2‐structure type. Instead it forms a layer‐like structure analogous to the well‐known barium compound Ba(H2O)6[B12H12]. Characteristic feature is the formation of isolated cation pairs [Li2(H2O)7]2+ in which the water molecules form two [Li(H2O)4]+ tetrahedra with eclipsed conformation, linked to a dimer via a common corner. The bridging oxygen atom (∢(Li‐ O ‐Li) = 112°) thereby formally substitutes Ba2+ in Ba(H2O)6[B12H12] according to (H2 O )Li2(H2O)6[B12H12]. A direct coordinative influence of the [B12H12]2— cluster anions to the Li+ cations is not noticeable, however. The positions of the hydrogen atoms of both the water molecules and the [B12H12]2— units have all been localized. In addition, the formation of B‐Hδ—···δ+H‐O‐hydrogen bonds between the water molecules and the hydrogen atoms from the anionic [B12H12]2— clusters is considered and their range and strength is discussed. The dehydratation of the heptahydrate has been investigated by DTA‐TG measurements and shown to take place in two steps at 56 and 151 °C, respectively. Thermal treatment leads to the anhydrous lithium dodecahydro‐closo‐dodecaborate Li2[B12H12], eventually. 相似文献
18.
Studies on Polyhalides. 11 Preparation and Crystal Structure of Diethylmethylphenylammoniumtriiodide, Et2MePhNI3 Diethylmethylphenylammoniumtriiodide C11H18NI3 crystallizes at room temperature monoclinically with a = 824.1(2) pm, b = 1 428.5(2) pm, c = 1 430.0(2) pm, β = 103.17(3)° and Z = 4. The crystal structure is build up from layers of the quarternary ammonium ions Et2MePhN+ and of the triiodide ions I3?, which alternate with each other along [1 0 0]. The packing of these layers and of the groups within each layer seems to be particularly effective without forming noticeable short contact distances. 相似文献
19.
Nd4N2Se3 and Tb4N2Se3: Two non‐isotypical Lanthanide(III) Nitride Selenides The non‐isotypical nitride selenides M4N2Se3 of neodymium (Nd4N2Se3) and terbium (Tb4N2Se3) are formed by the reaction of the respective rare‐earth metal with sodium azide (NaN3), selenium and the corresponding rare‐earth tribromide (MBr3) at 900 °C in evacuated silica ampoules after seven days. Each of them crystallizes monoclinically in the space group C2/c with Z = 4 for Nd4N2Se3 (a = 1300.47(4), b = 1009.90(3), c = 643.33(2) pm, β = 90.039(2)°) and in the space group C2/m with Z = 2 for Tb4N2Se3 (a = 1333.56(5), b = 394.30(2), c = 1034.37(4) pm, β = 130.377(2)°), respectively. The crystal structures differ fundamentally in the linkage of the structure dominating N3‐ centred (M3+)4 tetrahedra. In Nd4N2Se3, the [NNd4] units are edge‐linked to bitetrahedra which are cross‐connected to [N(Nd1)(Nd2)]3+ layers via their remaining four corners, whereas the [NTb4] tetrahedra in Tb4N2Se3 share cis‐oriented edges to form strands [N(Tb1)(Tb2)]3+. Both structures contain two crystallographically different M3+ cations, that show coordination numbers of six and seven (Nd4N2Se3) or twice six (Tb4N2Se3), respectively, relative to the anions (N3‐ und Se2‐). Each of the two independent kinds of Se2‐ anions provide the three‐dimensional linkage as well as the charge balance. The particular axial ratio a/c and the monoclinic reflex angle offer two choices for fixing the unit cell of Tb4N2Se3. 相似文献
20.
Preparation and Crystal Structure of the Tetramethylammonium Thiocyanate Sulfur Dioxide Adduct, (CH3)4N+SCN– · SO2 Tetramethylammonium thiocyanate reacts with sulfur dioxide under formation of tetramethylammonium thiocyanate sulfur dioxide adduct. The resulting salt is characterised by NMR and vibrational spectroscopy and its crystal structure. (CH3)4N+SCN– · SO2 crystallizes in the monoclinic space group P21/c with a = 578.4(1) pm, b = 1634.3(1) pm, c = 1054.6(1) pm, β = 105.17(1)°, and four formula units in the unit cell. The crystal structure possesses a strong S–S interaction between the NCS– anion and the SO2 molecule. The NCS–SO2 distance of 301.02(9) pm is longer than a covalent single bond, thus the compound is rather described as an adduct. The structure is compared with ab initio calculated data. 相似文献