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1.
Synthesis and Structure of a High Temperature Cobaltarsenate: H? Co3(AsO4)2 Single crystals of the high temperature compound H? Co3(AsO4)4 were prepared at 1800°C with a CO2-Laser technique. X-ray single crystal work shows monoclinic symmetry (space group C-P21/c; a = 6.457, b = 8.510, c = 11.187 Å; ß = 90.73°). In opposition to monoclinic m-CO3(AsO4)2 H? Co3(AsO4)2 has a different coordination of Co2+ including a different connection of the distorted polyhedra. There exists a significant similarity to Cu3(AsO4)2.  相似文献   

2.
The Crystal Chemistry of Copper Rare-Earth Oxotungstates: (I): triclinic-α-CuTbW2O8, (II): monoclinic-CuInW2O8 and (III): monoclinic-CuYW2O8 Single crystals of (I), (II) and (III) were prepared by recrystallisation in closed systems and examined by X-ray technique. (I): space group C? P1 , a = 7.3080, b = 7.8945, c = 7.1476 Å, α = 115.23, β = 116.21, γ = 56.98°, Z = 2; (II): space group C? C2/c, a = 9.6576, b = 11.6496, c = 4.9863 Å, β = 91.17°, Z = 4; (III): space group C? P2/n, a = 10.0504, b = 5.8214, c = 5.0224 Å, β = 94.23°, Z = 2. The crystal structures are discussed with respect to calculations of the coulombterms of lattice energy and possible valence states of Cu2+ and Mo5+.  相似文献   

3.
A Contribution about a New Cobalt-rich Oxoarsenate/-vanadate: Co5AsVO10 Single crystals of Co5AsVO10 were prepared by solid state reactions and investigated by X-ray structure determination. It crystallizes with monoclinic symmetry, space group C–C2/m, a = 19.134, b = 6.095, c = 17.482 Å, β = 133.37°; Z = 8. The new structure type is characterized by layers of CoO6- and AsO6-octahedra with partly alternating occupation. The layers are connected by Co2+ within tetrahedral oxygen coordination and tetrahedra around statistically occupied point positions of V5+ /As5+.  相似文献   

4.
Crystal Structure of CaZn2(OH)6 · 2 H2O The electrochemical oxidation of zinc in a zinc/iron-pair leads in an aqueous NH3 solution of calciumhydroxide at room temperature to colourless crystals of CaZn2(OH)6 · 2 H2O. The X-ray structure determination was now successful including all hydrogen positions. P21/c, Z = 2, a = 6.372(1) Å, b = 10.940(2) Å, c = 5.749(2) Å, β = 101.94(2)° N(F ≥ 3σF) = 809, N(Var.) = 69, R/RW = 0.011/0.012 The compound CaZn2(OH)6 · 2H2O contains Zn2+ in tetrahedral coordination by OH? and Ca2+ in octahedral coordination by four OH? and two H2O. The tetrahedra around Zn2+ form corner sharing chains, three-dimensionally linked by isolated polyhedra around Ca2+. Weak hydrogen bridge bonds result between H2O as donor and OH?.  相似文献   

5.
The Crystal Structure of Cu2M(BO3)O2 (M = Fe3+, Ga3+) Single Crystals of the compounds Cu2M(BO3)O2 (M = Fe3+ (I), Ga3+ (II)) were obtained by a B2O3 flux-technique. 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); I: a = 3.108(1); b = 12.003(1); c = 9.459(3) Å; b? = 96.66(3)°; Z = 4 and II: a = 3.1146(2); b = 11.921(3); c = 9.477(2) Å; b? = 97.91(2)°; Z = 4. All metal-sites are distorted octahedraly coordinated by oxygen-ions. The structure contains isolated planar BO3-units and oxygen which is not coordinated to boron.  相似文献   

6.
Synthesis and Crystal Structure of Sr2Zn(OH)6 and Ba2Zn(OH)6 Crystallization from supersaturated sodium hydroxozincate solutions by adding solutions of alkali earth metal hydroxides yields crystals of Sr2Zn(OH)6 and Ba2Zn(OH)6. The X-ray structure determination on these crystals was successful including all hydrogen positions: Sr2Zn(OH)6: P21/n, Z = 2, a = 5.794(1) Å, b = 6.160(1) Å, c = 8.141(1) Å, b = 91.23(1)°, N(F ³° 2σ F) = 1127, N(Var.) = 53, R1/wR2 = 0.047/0.081Ba2Zn(OH)6: P21/n, Z = 2, a = 6.043(1) Å, b = 6.336(1) Å, c = 8.451(2) Å, b = 91.23(2)°, N(F ° 2σ F) = 1669, N(Var.) = 54, R1/wR2 = 0.029/0.067. Sr2Zn(OH)6 and Ba2Zn(OH)6 crystallize isotypic in a distorted Li2O structure type. Sr2+ resp. Ba2+ form a cubic primitive arrangement. Distorted octahedra of OH around Zn2+ fill therein alternating cubic gaps in an ordered way.  相似文献   

7.
On the Crystal Structure of Ba2ZnO3 Single crystals of Ba2ZnO3 were prepared by solid state reaction. It crystallizes monoclinic: space group C ? C12/c1; a = 5.833; b = 11.376; c = 12.585 Å; β = 93.63°; Z = 8. The crystal structure is characterised by [ZnO3] chains along [100]. They are connected by Ba2+ in seven fold oxygen coordination.  相似文献   

8.
Preparation, Crystal Structures, Vibrational Spectra, and Normal Coordinate Analysis of [(Mo6Br )Y ]2?; Ya ? CN, NCS By treatment of [(Mo6Br)Bra6]2? with AgNO3 in acetone and addition of KCN or KNCS the hexacyano and hexaisothiocyanato derivates [(Mo6Br)Y]2?, Ya ? CN, NCS are formed. X-ray structure determinations of (Ph4P)2 [(Mo6Br)(CN)a6]·4H2 O ( 1 ) (triclinic, spacegroup P1, a = 11.63(3), b = 11.85(1), c = 14.23(5) Å, α = 71.8(1)°, β = 67.6(3)°, γ = 62.8(1)°, Z= 1) and (n-Bu4N)2[(Mo6Br i8)(NCS)a6] · 2Et2O ( 2 ) (monoclinic, spacegroup P21/n, a = 11.483(3), b = 16.348(5), c = 20.059(6) Å, β= 95.44(3)°, Z = 2) have been performed. The via C coordinated cyano ligands of ( 1 ) reveal facial groups with (MoCN) angles of 168.0–171,5° and 174.1°–175.7°. In ( 2 ) the via N coordinated isothiocyanato groups at the apical positions show MoNC-angles of 164.4°, the equatorial angles are 172.7–173.5°. Using the molecular parameters of the X-ray determinations the 10 K IR and Raman spectra of the (n-Bu4N) cluster salts are assigned by normal coordinate analyses based on a modified valence force field. The valence force constants are fd(MoMo) = 1.41 (CNa), 1.43 (NCSa), fd (MoBri) = 0.97 (CNa), 0.96 (NCSa), fd(MoC) = 1.62, fd(Mo-N) = 2.09 mdyne/Å.  相似文献   

9.
Tetraammine Lithium Cations Stabilizing Phenylsubstituted Zintl-Anions: The Compound [Li(NH3)4]2[Sn2Ph4] Ruby-red, brittle single crystals of [Li(NH3)4]2[Sn2Ph4] were synthesized by the reaction of diphenyltin dichloride and metallic lithium in liquid ammonia at ?35°C. The structure was determined from X-ray singlecrystal diffractometer data: Space group, P1 , Z = 1, a = 9.462(2) Å, b = 9.727(2) Å, c = 11.232(2) Å, α = 66.22(3)°, β = 85.78(3)°, γ = 61.83(3)°, R1 (F ? 4σF) = 5.13%, wR2 (F02 ? 4σF) = 10.5%, N(F ? 4σF) = 779, N(Var.) = 163. The compound contains to Sb2Ph4 isosteric centres [Sn2Ph4]2? as anions which are connected to rods by lithium cations in distorted tetrahedral coordination by ammonia. These rods are arranged parallel to one another in the b,c-plane, but stacked along [100].  相似文献   

10.
A New Structure Type of Copper Lanthanoide Oxotungstates: CuDy5(WO4)8 Single crystals of the hitherto unknown compound CuDy5(WO4)8 were prepared in closed copper tubes and investigated by X-ray technique. It shows monoclinic symmetry, space group C—C2/c, a = 19.118, b = 5.612, c = 11.518 Å, β = 111.32°, Z = 2. The crystal structure is characterized by [W4O18] groups which are connected to layers. Dy3+ shows one sided capped trigonal prisms and Cu+/Dy3+ with statistical distribution an octahedral oxygen surrounding.  相似文献   

11.
Synthesis, Crystal Structures, and Vibrational Spectra of [(Ph3P)2N]2[(W6Cl )I ] · 2 Et2O · 2 CH2Cl2 and [(Ph3P)2N]2[(W6Cl )(NCS) ] · 2 CH2Cl2 By treatment of [(W6Cl)I]2– with (SCN)2 in dichloromethane at –20 °C the hexaisothiocyanato cluster anion [(W6Cl)(NCS)]2– is formed. X‐ray structure determinations have been performed on single crystals of [(Ph3P)2N]2[(W6Cl)I] · 2 CH2Cl2 · 2 Et2O ( 1 ) (triclinic, space group P1, a = 10.324(5), b = 14.908(3), c = 17.734(8) Å, α = 112.78(2)°, β = 99.13(3)°, γ = 92.02(3)°, Z = 1) and [(Ph3P)2N]2[(W6Cl)(NCS)] · 2 CH2Cl2 ( 2 ) (triclinic, space group P1, a = 11.115(2), b = 14.839(2), c = 17.036(3) Å, α = 104.46(1)°, β = 105.75(2)°, γ = 110.59(1)°, Z = 1). The thiocyanate ligands of 2 are bound exclusively via N atoms with W–N bond lengths of 2.091–2.107 Å, W–N–C angles of 173.1–176.9° and N–C–S angles of 178.1–179.3°. The vibrational spectra exhibit characteristic innerligand vibrations at 2067–2045 (νCN), 879–867 (νCS) and 490–482 (δNCS). Based on the molekular parameters of the X‐ray determination of 1 the vibrational spectra of the corresponding (n‐Bu4N) salt of 1 are assigned by normal coordinate analysis. The valence force constants are fd(WW) = 1.61, fd(WI) = 1.23 and fd(WCl) = 1.10 mdyn/Å.  相似文献   

12.
Nitride Sulfide Chlorides of the Lanthanides. III. Synthesis and Crystal Structure of Pr5N3S2Cl2 By reacting praseodymium with sulfur, sodium azide and praseodymium trichloride in sealed, evacuated silica tubes (850°C, 7 d), the nitride sulfide chloride Pr5N3S2Cl2 is obtained in case of a 4:2:1:1 molar ratio of the reactants (Pr:S:NaN3:PrCl3). A slight excess of trichloride or the addition of NaCl as a flux supports the yield of brownish red, rod-shaped transparent crystals which prove to be stable against hydrolysis. The crystal structure (monoclinic, C2/m (no. 12), a = 1540.2(1), b = 400.92(3), c = 1656.3(1) pm, β = 101.24(1)°, Z = 4, R = 0.039, Rw = 0.028) was determined by means of X-ray single crystal data. Thus five crystallographically different cations (Pr3+) are present which with three distinct kinds of nitride anions (N3?) build up two types of translationally commensurate chains from interconnected [NPr4] tetrahedra. With an additional edge per “chain-link” in chain I, two single chains [NPr3/3ePr1/1t]3+ (?[NPr2]3+) of cis-edge connected [NPr4] tetrahedra (known from the Sm4N2S3-type structure) are condensed into the double chain [(N1){(Pr1)(2+2)/(2+2)e,e(Pr2)(2+1)/(2+1)e,v}(N2)(Pr3)1/1t]3+ (?[N2Pr3]3+). Chain II consists of two single chains [NPr2/2vPr2/1t] 6+ (?[NPr3]6+) of vertex-connected [NPr4] tetrahedra (known from the Sm3NS3-type structure), which are condensed to the double chain [(N3)(Pr4)2/2e(Pr5)2/2v]3+ (?[NPr2]3+) via an additional edge per “chain-link” too. Both types of chains are bundled along [010] like a closest packing of rods. Four crystallographically different but by X-ray diffraction indistinguishable anions S2? and Cl? hold both cationic double chains together and also adjust the charge balance in a molar ratio of 1 : 1.  相似文献   

13.
LaCl(BO2)2 and Er2Cl2[B2O5]: Two Chloride Oxoborates of Trivalent Lanthanides Er2Cl2[B2O5] is obtained as single crystals by the reaction of ErCl3, Er2O3 and B2O3 with an excess of ErCl3 as flux in evacuated silica tubes after two weeks at 850 °C. The compound crystallizes as long, pale pink needles and appears to be air‐ and water‐resistant. Single‐crystalline LaCl(BO2)2 emerges from the reaction of La2O3, LaCl3, and B2O3 with an excess of B2O3 as flux in evacuated silica tubes after four weeks at 900 °C. LaCl(BO2)2 crystallizes as thin, colourless, air‐ and water‐resistant needles which tend to severe twinning due to their fibrous habit. The crystal structure of Er2Cl2[B2O5] (orthorhombic, Pbam; a = 1489.65(9), b = 1004.80(6), c = 524.86(3) pm; Z = 4) contains two crystallographically different erbium cations. (Er1)3+ resides in pentagonal‐bipyramidal coordination of seven anions while (Er2)3+ is surrounded by only six anions with the shape of an octahedron. The planar oxodiborate units [B2O5]4— consisting of two vertex‐shared [BO3]3— triangles are isolated according to {([BOO]2)4—}. LaCl(BO2)2 crystallizes isostructurally with PrCl(BO2)2 in the triclinic space group P1¯ (a = 423.52(4), b = 662.16(7), c = 819.33(8) pm; α = 82.081(8), β = 89.238(9), γ = 72.109(7)°; Z = 2). The characteristic unit consists of endless chains built up by corner‐linked [BO3]3— triangles. These quasi‐planar zigzag chains of the composition {[(B1)OO(B2)OO]2—} (≡ {[BO2]} run parallel [100]. The La3+ cations exhibit coordination numbers of ten and are coordinated by three Cl and seven O2— anions.  相似文献   

14.
Synthesis, Crystal Structures, and Vibrational Spectra of [(Mo6X)Y]2–; Xi = Cl, Br; Ya = NO3, NO2 By treatment of [(Mo6X)Y]2–; Xi = Ya = Cl, Br with AgNO3 or AgNO2 by strictly exclusion of oxygene in acetone the hexanitrato and hexanitrito cluster anions [(Mo6X)Y]2–, Ya = NO2, NO3 are formed. X-ray structure determinations of (Ph4As)2[(Mo6Cl)(NO3)] · 2 Me2CO ( 1 ) (monoclinic, space group P21/n, a = 12.696(3), b = 21.526(1), c = 14.275(5) Å, β = 115.02(2)°, Z = 2), (n-Bu4N)2[(Mo6Br)(NO3)] · 2 CH2Cl2 ( 2 ) (monoclinic, space group P21/n, a = 14.390(5), b = 11.216(5), c = 21.179(5)Å, β = 96.475(5)°, Z = 2) and (Ph4P)2[(Mo6Cl)(NO2)] (3) (monoclinic, space group P21/n, a = 11.823(5), b = 13.415(5), c = 19.286(5) Å, β = 105.090(5)°, Z = 2) reveal the coordination of the ligands via O atoms with (Mo–O) bond lengths of 2.11–2.13 Å, and (MoON) angles of 122–131°. The vibrational spectra of the nitrato compounds show the typical innerligand vibrations νas(NO2) (∼ 1500), νs(NO2) (∼ 1270) and ν(NO) (∼ 980 cm–1). The stretching vibrations ν(N=O) at 1460–1490 cm–1 and ν(N–O) in the range of 950–1000 cm–1 are characteristic for nitrito ligands coordinated via O atoms.  相似文献   

15.
Synthesis, Crystal Structures, and Vibrational Spectra of [OsCl(acac)(EPh3)], E = P, As, Sb By reaction of tetrachloroacetylacetonatoosmate(IV) with PPh3, AsPh3 or SbPh3 in ethanol the complexes [OsCl(acac)(EPh3)], E = P, As, Sb are formed, which are purified by chromatography on silica gel. X-ray crystal structure determinations of the isotypic single crystals of [OsCl(acac)(EPh3)] (monoclinic, space group P 21/c, Z = 4; E = P ( 1 ): a = 12.972(2), b = 18.255(2), c = 16.517(2) Å, β = 112.61(2)°; E = As ( 2 ): a = 13.173(5), b = 18.299(5), c = 16.429(5) Å, β = 112.346(5)°; E = Sb ( 3 ): a = 13.573(3), b = 18.520(3), c = 16.440(9) Å, β = 111.78(2)°) result in mean bond distances Os–P = 2.412, Os–As = 2.485, Os–Sb = 2.619, Os–Cl = 2.354 and Os–O = 2.032 Å. The IR spectra (10 K) exhibit the inner ligand vibrations of the acac and EPh3 groups with nearly constant frequencies and the stretching vibrations of OsP at 500–524, of OsAs at 330–339, of OsSb at 271–278, of OsCl at 317–322 and of Os–O in the range 460–694 cm–1.  相似文献   

16.
Cs[Er10(C2)2]I18 and [Er10(C2)2]Br18: Two New Examples for Reduced Halides of the Lanthanides with Isolated [M10(C2)2] Clusters Cs[Er10(C2)2]I18 is obtained from the reaction of ErI3 with caesium and carbon in sealed tantalum containers at 700°C and [Er10(C2)2]Br18 through the metallothermic reduction of ErBr3 with rubidium in the presence of carbon at 750°C in sealed niobium containers. The crystal structures {Cs[Er10(C2)2]I18: triclinic, P1 ; a = 1 105.2(8) pm, b = 1 112.0(7) pm; c = 1 122.9(8) pm; α = 66.91(3)°, β = 87.14(3)°; γ = 60.80(3)°; Z = 1; R = 0.049, Rw = 0.043; [Er10(C2)2]Br18: monoclinic, P21/n, a = 971.8(6) pm, b = 1 623.4(9) pm, c = 1 163.8(6) pm, β = 104.00(6)°; Z = 2; R = 0.077, Rw = 0.057} contain isolated dimeric [Er10(C2)2] clusters. Due to the inclusion of C2 units, the octahedra are elongated in the direction of the pseudo C4 axis. The connecting edges of the two octahedra are exceptionally short (316.7 pm and 314.8 pm respectively). The dimeric units are connected via Xi?a and Xa?i (X = Br, I) bridges according to [Er10(C2)2XX]X. Cs+ is surrounded by a cuboctahedron of iodide ions in Cs[Er10(C2)2]I18.  相似文献   

17.
Lithium Triamidostannate(II), Li[Sn(NH2)3] – Synthesis and Crystal Structure Rusty-red glistening, transparent crystals of Li[Sn(NH2)3] were obtained by reaction of metallic lithium with tetraphenyl tin in liquid ammonia at 110 °C. The structure was determined from X-ray single-crystal diffractometer data: Space group P 21/n, Z = 4, a = 8.0419(9) Å, b = 7.1718(8) Å, c = 8.5085(7) Å, β = 90.763(8)°, R1 (F o ≥ 4σ(F o)) = 2.8%, wR2 (F ≥ 2σ(F )) = 5.3%, N(F ≥ 2σ(F )) = 1932, N(Var.) = 65. The crystal structure contains trigonal pyramidal complex anions [Sn(NH2)3] with tin at the apex, which are connected to layers of sequence A B A B … by lithium in tetrahedra-double units [Li(NH2)2/2(NH2)2]2.  相似文献   

18.
Synthesis, Crystal Structures, and Vibrational Spectra of [OsBr(acac)(PPh3)] and [OsBr(acac)(AsPh3)] By reaction of tetrabromoacetylacetonatoosmate(IV) with PPh3 or AsPh3 in ethanol the complexes [OsBr(acac)(PPh3)] ( 1 ) and [OsBr(acac)(AsPh3)] ( 2 ) are formed, which are purified by chromatography on silica gel. X-ray structure determinations of single crystals of ( 1 ) (monoclinic, space group P 21/n, a = 13.035(2), b = 18.2640(14), c = 16.636(3) Å, β = 112.776(14)°, Z = 4) and ( 2 ) (monoclinic, space group P 21/c, a = 13.23(5), b = 18.35(2), c = 16.65(2) Å, β = 112.9(5)°, Z = 4) result in mean bond distances Os–P = 2.413, Os–As = 2.483, Os–Br = 2.488 and Os–O = 2.037 Å. The vibrational spectra (10 K) exhibit the inner ligand vibrations of the acac, PPh3 and AsPh3 groups with nearly constant frequencies and the stretching vibrations of OsP at 499–522, of OsAs at 330–339, of OsBr at 213–214 and of OsO in the range 460–694 cm–1.  相似文献   

19.
Na2BaCuV2O8: A New Structure Type of the Alkaline-Alkaline Earth Copper Oxovanadates Single crystals of Na2BaCuV2O8 were prepared by a high temperature flux. It crystallizes with monoclinic symmetry space group C–C2/c, a = 9.4329 Å, b = 5.6858 Å, c = 14.0488 Å, β = 92.344° Z = 4 and represents a new structure type. The crystal structure show VO4 tetrahedra, stretched CuO6 octahedra, trigonal bipyramids around Na+ and a BaO10+2 polyedron.  相似文献   

20.
[Li(THF)4][[NN]2Nd2Cl25-O)Li3] ( 2 ) ([NN]3– = ([Me3SiNCH2CH2)3N]3–) was prepared by transmetallation of Li3[NN] with anhydrous neodymium trichloride in THF. After recrystallization from diethylether/pentane (1 : 2) light blue crystals of 2 were obtained, which were characterized by single crystal X-ray diffraction. Space group: P21/n, Z = 4, lattice dimensions at 203 K: a = 1260.8(3), b = 3832.5(8), c = 1569.2(3) pm, β = 106.07(3)°, R1 = 0.0541. In the anion of 2 a nearly trigonal bipyramidal [Nd2Li35-O)]7+ unit is observed.  相似文献   

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