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1.
The crystal structure of the title compound, {(C3H12N2)[Mo3O10]·2H2O}n, is composed of [Mo3O10]2− anionic chains, propane‐1,3‐diammonium cations and solvent water molecules. The [Mo3O10]2− chain is constructed from edge‐sharing MoO6 octahedra. The protonated propane‐1,3‐diamine cations and solvent water molecules are located between the chains and are linked to the O atoms of the inorganic chains by hydrogen bonds.  相似文献   

2.
In the title compound, (C6H8N4)[AuCl4]Cl, the 4,4′‐bi(1H‐pyrazol‐2‐ium) dication, denoted [H2bpz]2+, is situated across a centre of inversion, the [AuCl4] anion lies across a twofold axis passing through Cl—Au—Cl, and the Cl anion resides on a twofold axis. Conventional N—H...Cl hydrogen bonding [N...Cl = 3.109 (3) and 3.127 (3) Å, and N—H...Cl = 151 and 155°] between [H2bpz]2+ cations (square‐planar node) and chloride anions (tetrahedral node), as complementary donors and acceptors of four hydrogen bonds, leads to a three‐dimensional binodal four‐connected framework with cooperite topology (three‐letter notation pts). The framework contains channels along the c axis housing one‐dimensional stacks of square‐planar [AuCl4] anions [Au—Cl = 2.2895 (10)–2.2903 (16) Å; interanion Au...Cl contact = 3.489 (2) Å], which are excluded from primary hydrogen bonding with the [H2bpz]2+ tectons.  相似文献   

3.
In the structure of the complex of dibenzo‐18‐crown‐6 [systematic name: 2,5,8,15,18,21‐hexaoxatricyclo[20.4.0.09,14]hexacosa‐1(26),9,11,13,22,24‐hexaene] with 4‐methoxyanilinium tetrafluoroborate, C7H10NO+·BF4·C20H24O6, the protonated 4‐methoxyanilinium (MB‐NH3+) cation forms a 1:1 supramolecular rotator–stator complex with the dibenzo‐18‐crown‐6 molecule via N—H...O hydrogen bonds. The MB‐NH3+ group is attached from the convex side of the bowl‐shaped crown, in contrast with similar ammonium cations that nest in the curvature of the bowl. The cations are associated via C—H...π interactions, while the cations and anions are linked by weak C—H...F hydrogen bonds, forming cation–crown–anion chains parallel to [011].  相似文献   

4.
Structure and Magnetic Properties of Bis{3‐amino‐1,2,4‐triazolium(1+)}pentafluoromanganate(III): (3‐atriazH)2[MnF5] The crystal structure of (3‐atriazH)2[MnF5], space group P1, Z = 4, a = 8.007(1) Å, b = 11.390(1) Å, c = 12.788(1) Å, α = 85.19(1)°, β = 71.81(1)°, γ = 73.87(1)°, R = 0.034, is built by octahedral trans‐chain anions [MnF5]2– separated by the mono‐protonated organic amine cations. The [MnF6] octahedra are strongly elongated along the chain axis (<Mn–Fax> 2.135 Å, <Mn–Feq> 1.842 Å), mainly due to the Jahn‐Teller effect, the chains are kinked with an average bridge angle Mn–F–Mn = 139.3°. Below 66 K the compound shows 1D‐antiferromagnetism with an exchange energy of J/k = –10.8 K. 3D ordering is observed at TN = 9.0 K. In spite of the large inter‐chain separation of 8.2 Å a remarkable inter‐chain interaction with |J′/J| = 1.3 · 10–5 is observed, mediated probably by H‐bonds. That as well as the less favourable D/J ratio of 0.25 excludes the existence of a Haldene phase possible for Mn3+ (S = 2).  相似文献   

5.
The complexes [Cu(AMTTO)Cl2] ( 2 ), [Cu(AMTTO)2]Cl ( 3 ), and [Cu(AMTTO)(PPh3)2Cl] ( 4 ) have been prepared and characterized by IR spectroscopy and elemental analyses. Also single‐crystal X‐ray diffraction studies on compound 2 , 3 and 4 revealed that AMTTO acts in 2 as a bidentate ligand via nitrogen and sulfur atoms, in 3 and 4 as a monodentate via sulfur atoms. Complex 3 was already mentioned in literature, but the structure was not described in detail. The molecules in 2 form infinite chains through additional weak Cu—S interactions along [010] indicating the Jahn‐Teller distortion of the d9 ion Cu2+. The infinite chains are connected by hydrogen bonding along [100]. Crystal data for 2 at —80°C: monoclinic, space group P21/m, a = 666.7(1), b = 609.4(1), c = 1132.6(2) pm, b = 95.46(2)°, Z = 2, R1 = 0.0365; for 3 at —80°C: orthorhombic, space group Pbcn, a = 1291.2(2), b = 1146.5(1), c = 1000.5(1) pm, Z = 4, R1 = 0.0315; for 4 at —80°C: monoclinic, space group, P21/n, a = 879.4(1), b = 1849.3(2), c = 2293.8(3) pm, β = 92.38(1)°, Z = 4, R1 = 0.0688.  相似文献   

6.
X‐ray data were obtained for the monoclinic polymorph of rac‐5,7,7,12,12,14‐hexa­methyl‐1,4,8,11‐tetraazonia­cyclo­tetra­decane bis­(hexa­fluoro­germanate) tetrahydrate, (C16H40N4)[GeF6]2·4H2O. The tetra­aza‐macrocyclic cations lie across inversion centers in space group P21/c. Water mol­ecules and [GeF6]2− anions form zigzag chains, which alternate in a three‐dimensional network with the macrocyclic cations. The structure is sustained by multiple hydrogen bonds.  相似文献   

7.
Crystal Structures of „Supramolecular”︁ Benzo‐18‐crown‐6 Potassium Tetrathiocyanato Metallates: A Dimeric Complex {[K(Benzo‐18‐crown‐6)]2[Hg(SCN)4]}2 and Two Isomeric Complexes [K(Benzo‐18‐crown‐6)][Cd(SCN)3] Containing Trithiocyanato Cadmate Anions with Chain Structures By reaction of potassium thiocyanatomercurate(II) complexes with benzo‐18‐crown‐6 (2,3‐benzo‐1,4,7,10,13,16‐hexaoxacyclooctadec‐2‐ene) crystals of {[K(benzo‐18‐crown‐6)]2[Hg(SCN4)]}2 ( 1 ) were obtained. 1 crystallizes monoclinic, space group P21/n (non‐standard setting of P21/c), a = 1737.35(2), b = 1377.16(2), c = 1984.12(3) pm, β = 100.637(1)°, Z = 2. With potassium tetrathiocyanatocadmate(II) two modifications of a complex [K(benzo‐18‐crown‐6)][Cd(SCN)3] ( 2 , 3 ), of different symmetry were formed. 2 crystallizes monoclinic, P21/c, a = 1158,31(3), b = 1096,55(2), c = 2028,46(2) pm, β = 99,5261(2)°, Z = 4, 3  orthorhombic, P21cn, a = 1105,95(3), b = 1413,07(4), c = 1617,10(5) pm, Z = 4. 1 has a dimeric structure, built up from a dication K2(benzo‐18‐crown‐6)2]2+ and two [K(benzo‐18‐crown‐6)]+ cations, which are bridged by two [Hg(SCN)4]2– anions. In 2 and 3 triply bridged infinite [{Cd(SCN)3}n] zigzag chains, stretching along screw axes, are to be found as anions. In 2 these chains exist in two conformations related by inversion symmetry, whereas in 3 only one form can be found. [K(benzo‐18‐crown‐6)]+ cations are linked to the anion chains via K · · · S interactions of different lengths.  相似文献   

8.
Production and Decomposition of (NH4)[BF4] and H3N‐BF3 (NH4)[BF4] is produced as single crystals during the reaction of elemental boron and NH4HF2 (B : NH4HF2 = 1 : 2) and NH4F (B : NH4F = 1 : 4), respectively, in sealed copper ampoules at 300 °C. The crystal structure (baryte type, orthorhombic, Pnma, Z = 4) was redetermined at ambient temperature (a = 909.73(18), b = 569.77(10), c = 729.47(11) pm, Rall = 0.0361) and at 140 K (a = 887.3(2), b = 574.59(12), c = 717.10(12) pm, Rall = 0.0321). Isolated (NH4)+ and [BF4] tetrahedra are the important building units. The thermal behaviour of (NH4)[BF4] was investigated under inert (Ar, N2) and reactive conditions (NH3) with the aid of DTA/TG and DSC measurements and with in‐situ X‐ray powder diffraction as well. Finally, (NH4)[BF4] is decomposed yielding NH3 and BF3, BN is not produced under the current conditions. Colourless single crystals of H3N‐BF3 were prepared directly from the components NH3 and BF3. The crystal structure was determined anew at 293 and 170 K (orthorhombic, Pbca, Z = 8, a = 815.12(10), b = 805.91(14), c = 929.03(12) pm, Rall = 0.0367; a = 807.26(13), b = 800.48(10), c = 924.31(11) pm, Rall = 0.0292, T = 170 K). The crystal structure contains isolated molecules H3N‐BF3 in staggered conformation with a B‐N distance of 158 pm. The thermal behaviour of H3N‐BF3 was studied likewise.  相似文献   

9.
Diorganoindium Cations. The Crystal Structure of [Mes2In][BF4] (PhCH3)2In and Mes3In react with BF3 · OEt2 in a ratio of 3:4 at 80°C in toluene to the corresponding salts [R2In][BF4] [R = PhCH2 ( 1 ), Mes ( 2 )]. The same results could be obtained, when the diorganoindium fluorides (PhCH2)2InF and Mes2InF were treated with BF3 · OEt2 at 80°C in toluene. 1 und 2 were characterized by NMR-, IR- und MS-techniques. The arrangement of the ions in 2 could be established by an X-ray structure determination. The cations and anions of 2 are forming infinite chains. The metal centers are coordinated by two BF4?-ions, so that every In atom possesses a distorted octahedral coordination sphere.  相似文献   

10.
New Copper Complexes Containing Phosphaalkene Ligands. Molecular Structure of [Cu{P(Mes*)C(NMe2)2}2]BF4 (Mes* = 2,4,6‐tBu3C6H2) Reaction of equimolar amounts of the inversely polarized phosphaalkene tBuP=C(NMe2)2 ( 1a ) and copper(I) bromide or copper(I) iodide, respectively, affords complexes [Cu3X3{μ‐P(tBu)C(NMe2)2}3] ( 2 ) (X =Br) and ( 3 ) (X = I) as the formal result of the cyclotrimerization of a 1:1‐adduct. Treatment of 1a with [Cu(L)Cl] (L = PiPr3; SbiPr3) leads to the formation of compounds [CuCl(L){P(tBu)C(NMe2)2}] ( 4a ) (L = PiPr3) and ( 4b ) (L = SbiPr3), respectively. Reaction of [(MeCN)4Cu]BF4 with two equivalents of PhP=C(NMe2)2 ( 1b ) yields complex [Cu{P(Ph)C(NMe2)2}2]BF4 ( 5b ). Similarly, compounds [Cu{P(Aryl)C(NMe2)2}2]BF4 ( 5c (Aryl = Mes and 5d (Aryl = Mes*)) are obtained from ArylP=C(NMe2)2 ( 1c : Aryl = Mes; 1d : Mes*) and [(MeCN)4Cu]BF4 in the presence of SbiPr3. Complexes 2 , 3 , 4a , 4b , and 5b‐5d are characterized by means of elemental analyses and spectroscopy (1H‐, 13C{1H}‐, 31P{1H}‐NMR). The molecular structure of 5d is determined by X‐ray diffraction analysis.  相似文献   

11.
A New Rare‐Earth Metal(III) Fluoride Oxoselenate(IV): YF[SeO3] Just two representatives of the rare‐earth metal(III) fluoride oxoselenates(IV) with the formula type MF[SeO3] (M = La and Lu) exist so far, whereas for the intermediate lanthanoids only M3F[SeO3]4‐type compounds (M = Gd and Dy) were accessible. Because of the similar radius of Y3+ to the radii of the heavier lanthanoid cations, a missing link within the MF[SeO3] series could be synthesized now with the example of yttrium(III) fluoride oxoselenate(IV). Contrary to LuF[SeO3] with its triclinic structure, YF[SeO3] crystallizes monoclinically in space group P21/c (no. 14, a = 657.65(7), b = 689.71(7), c = 717.28(7) pm, β = 99.036(5)° and Z = 4). A single Y3+ cation occupying the general site 4e is surrounded by six oxide and two fluoride anions forming [YO6F2]11? polyhedra (d(Y–O) = 228–243 plus 263 pm, d(Y–F) = 219–220 pm). These are linked via common O···O edges to chains running along [010] and adjacent chains get tied to each other by sharing common O3···O3 and O3···F edges which results in sheets parallel to (100). The Se4+ cations connect these sheets as ψ1‐tetrahedral [SeO3]2? anions (d(Se–O) = 168–174 pm) for charge balance via all oxygen atoms. Despite the different coordination numbers of seven and eight for the rare‐earth metal(III) cations the structures of LuF[SeO3] and YF[SeO3] appear quite similar. The chains containing pentagonal bipyramids [LuO5F2]9? are connected to layers running parallel to the (100) plane again. In fact it is only necessary to shorten the partial structure of the straight chains along [001] to achieve the angular chains in YF[SeO3]. As a result of this shortening one oxide anion at a time moves into the coordination sphere of a neighboring Y3+ cation and therefore adds up the coordination number for Y3+ to eight. For the synthesis of YF[SeO3] yttrium sesquioxide (Y2O3), yttrium trifluoride (YF3) and selenium dioxide (SeO2) in a molar ratio of 1 : 1 : 3 with CsBr as fluxing agent were reacted within five days at 750 °C in evacuated graphitized silica ampoules.  相似文献   

12.
The title novel manganese(II) coordination polymer, {(C10H10N2)[MnCl4]}n, consists of a one‐dimensional infinite zigzag chain composed of polymeric [MnCl4]2− units in which each Mn2+ ion is located on a twofold rotation axis and is coordinated to two terminal Cl atoms and four bridging chloro ligands. Adjacent Mn2+ ions are linked by double Cl bridges arranged about a centre of inversion, thus forming anionic chains of distorted edge‐sharing octa­hedra. Rows of approximately parallel 4,4′‐bipyridinium cations run side‐by‐side with the MnCl4 chains. A two‐dimensional layer structure is constructed via hydrogen bonds and by additional π–π stacking inter­actions.  相似文献   

13.
(C2H10N2)[BPO4F2] — Strukturbeziehungen zwischen [BPO4F2]2— und [Si2O6]4— Colourless crystals of (C2H10N2)[BPO4F2] were prepared from mixture of ethylendiamine, H3BO3, BF3 · C2H5NH2, H3PO4 and HCl under mild hydrothermal conditions (220 °C). The crystal structure was determined by single crystal methods (triclinic, P1¯ (no. 2), a = 451.85(5) pm, b = 710.20(8) pm, c = 1210.2(2) pm, α = 86.08(1)°, β = 88.52(2)°, γ = 71.74(1)°, Z = 2) and contains infinite tetrahedral zweier‐single‐chains {[BPO4F2]2—} which are isoelectronic (48e) with the polyanions {[Si2O6]4—} of the pyroxene family.  相似文献   

14.
The title compound, [Cu{N(CN)2}(C12H8N2)2]BF4, was prepared as part of our study of the shape of coordination polyhedra in five‐coordinated copper(II) complexes. Single‐crystal X‐ray analysis reveals that the structure consists of [Cu{N(CN)2}(phen)2]+ cations (phen is 1,10‐phenanthroline) and BF4 anions. The Cu centre is five‐coordinated in a distorted trigonal bipyramidal manner by four N atoms of two phen ligands and one N atom of a dicyanamide anion, which is coordinated in the equatorial plane at a distance of 1.996 (2) Å. The two axial Cu—Nphen distances have similar values [average 1.994 (6) Å] and are shorter than the two equatorial Cu—Nphen bonds [average 2.09 (6) Å]. This work demonstrates the effect of ligand rigidity on the shape of coordination polyhedra in five‐coordinated copper(II) complexes.  相似文献   

15.
La3OCl[AsO3]2: A Lanthanum Oxide Chloride Oxoarsenate(III) with a “Lone‐Pair” Channel Structure La3OCl[AsO3]2 was prepared by the solid‐state reaction between La2O3 and As2O3 using LaCl3 and CsCl as fluxing agents in evacuated silica ampoules at 850 °C. The colourless crystals with pillar‐shaped habit crystallize tetragonally (a = 1299.96(9), c = 558.37(5) pm, c/a = 0.430) in the space group P42/mnm (no. 136) with four formula units per unit cell. The crystal structure contains two crystallographically different La3+ cations. (La1)3+ is coordinated by six oxygen atoms and two chloride anions in the shape of a bicapped trigonal prism (CN = 8), whereas (La2)3+ carries eight oxygen atoms and one Cl? anion arranged in the shape of tricapped trigonal prism (CN = 9). The isolated pyramidal [AsO3]3? anions (d(As–O) = 175–179 pm) consist of three oxygen atoms (O2 and two O3), which surround the As3+ cations together with the free, non‐binding electron pair (lone pair) Ψ1‐tetrahedrally (?(O–As–O) = 95°, 3×). One of the three crystallographically independent oxygen atoms (O1), however, is exclusively coordinated by four (La2)3+ cations in the shape of a real tetrahedron (d(O–La) = 236 pm, 4×). These [(O1)(La2)4]10+ tetrahedra form endless chains in the direction of the c axis through trans‐edge condensation. Empty channels, constituted by the lonepair electrons of the Cl? anions and the As3+ cations in the Ψ1‐tetrahedral oxoarsenate(III) anions [AsO3]3?, run parallel to [001] as well.  相似文献   

16.
The crystal structures of the title compounds, (C2N3H8)2[CuCl4], (I), and (C8H14N4)[CuCl4], (II), have been studied by X‐ray diffraction. The structures consist of discrete [CuCl4]2? anions with two monoprotonated (C2N3H8)+ cations for (I) and a diprotonated (C8N4H14)2+ cation for (II). The [CuCl4]2? anions of both compounds have flattened tetrahedral geometries. There are several N—H?Cl weak bonds that join the [CuCl4]2? anions and the organic cations helping retain the pseudo‐tetrahedral geometries of the anions.  相似文献   

17.
The structures of the title complexes, (C6H15N2)2[MoS4], (I), and (C6H16N2)[MoS4], (II), can be described as consisting of discrete tetra­hedral [MoS4]2− dianions that are linked to the organic ammonium cations via weak hydrogen‐bonding inter­actions. The asymmetric unit of (I) consists of a single (±)‐trans‐2‐amino­cyclo­hexyl­ammonium cation in a general position and an [MoS4]2− anion located on a twofold axis, while in (II), two crystallographically independent trans‐cyclo­hexane‐1,4‐diammonium cations located on centres of inversion and one [MoS4]2− anion in a general position are found. The differing dispositions of the amine functionalities in the organic cations in the title complexes lead to different crystal packing arrangements in (I) and (II).  相似文献   

18.
In the title compound, catena‐poly[diselanylbis(1,3‐dimethyl‐1H‐imidazol‐3‐ium) [μ3‐chlorido‐tetra‐μ2‐chlorido‐tricuprate(I)]], {(C10H16N4Se2)[Cu3Cl5]}n, the diselenide dication is stabilized by catena‐[Cu3Cl5]2− anions which associate through strong Cu—Cl bonds [average length = 2.3525 (13) Å] to form polymeric chains. The polymeric [Cu3Cl5]2− anion contains crystallographically imposed twofold rotation symmetry, with distorted trigonal‐planar and tetrahedral geometries around the two symmetry‐independent Cu atoms. Likewise, the Se—Se bond of the cation is centered on a twofold rotation axis.  相似文献   

19.
Sr2(OLi2Sr4)[CrN4]2, a Nitridochromate(VI)‐Oxide with Oxygen in Tetragonal‐Bipyramidal Coordination by Lithium and Strontium Green gleaming crystals of Sr2(OLi2Sr4)[CrN4]2 were prepared by reaction of Li, Sr and CrN/Cr2N (approximate 1 : 1 mixture) with flowing nitrogen at 900 °C (molar overall composition Li : Sr : Cr = 6 : 1 : ∼3). The oxygen content results from a leak in the gas supply. The crystal structure was determined by single crystal methods (triclinic; P1; a = 615.87(9) pm, b = 682.50(10) pm, c = 754.30(8) pm, α = 82.302(14)°, β = 75.197(10)°, γ = 70.133(13)°; Z = 1) and contains distorted tetragonal bipyramids (OLi2Sr4)8+ and [CrVIN4]6–‐tetrahedra besides Sr2+.  相似文献   

20.
The title compound, {(C6H14N2O2)[Cu2Cl6(H2O)]}n, consists of 1,4‐dihydroxy‐1,4‐diazoniabicyclo[2.2.2]octane dications and one‐dimensional inorganic anionic {[Cu2Cl6(H2O)]2−}n chains in which both five‐coordinate [CuCl3(H2O)] and five‐coordinate [CuCl3] units exist. These two distinct type of unit are linked together by one chloride ion and are bridged across centres of inversion to further units of their own type through two chloride ions, giving rise to novel polymeric zigzag chains parallel to the c axis. The chains are connected by O—H...Cl hydrogen bonds to produce R24(16) ring motifs, resulting in two‐dimensional layers parallel to the ac plane. These layers are linked into a three‐dimensional framework with the organic cations via O—H...Cl hydrogen bonds. Hydrogen bonding between the chains, and between the chains and the organic cations, provides stability to the crystal structure.  相似文献   

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