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1.
Rubidium Hexaamidolanthanate and -neodymate, Rb3[La(NH2)6] and Rb3[Nd(NH2)6]; Compounds. Structurally Related to K3[Cr(OH)6] and K4CdCl6 Colourless Rb3[La(NH2)6] (a = 12.298(4) Å, c = 13.759(2) Å, N = 6, R3 c) and pale blue Rb3[Nd(NH2)6] (a = 12.199(6) Å, c = 13.626(4) Å, N = 6, R32) have been prepared by the reaction of the corresponding metals (Rb: La resp. Nd = 3:1) with NH3(P(NH3) = 4–4.5 kbar) at 300°C. Single crystal x-ray methods gave their structures. It is shown by space group relations that these compounds are structurally related to one another and to further ternary amides as well as to K3[Cr(OH)6] and K4CdCl6. 相似文献
2.
News on K2[MnF6], Rb2[MnF6], and Cs2[MnF6] Cs2[MnF6] (a = 8.972 Å) and Rb2[MnF6] (a = 8.531 Å) as well as this with K2[MnF6] (a = 8.221 Å and hexagonal a = 5.722, c = 9.331 Å) form mixed crystals of the K2PtCl6 type of structure. Calculations of the Madelung Part of Lattice Energy, MAPLE, and Effective Coordination Numbers, ECoN, lead contrary to former assumptions to distances Mn? F of about 1.86 Å (CN 6). 相似文献
3.
New Oxogallates of Alkaline Metals: On K6[Ga2O6] and Rb6[Ga2O6] as well as Na3GaO3 and Cs6[Ga2O6] Due to powder and single crystal data K6[Ga2O6] a = 7.099; b = 11.116; c = 6.484 Å; ß = 101.66° and Rb6[Ga2O6] a = 7.393; b = 11.475; c = 6.798 Å; ß = 103.5° crystallize isotypic with K6[Fe2O6]; space group C2/m-C32h; As well has been prepared the hitherto unknown Na3GaO3 a = 11.48, b = 10.82, c = 6.13 Å, space-group Imcm or I2cm Z = 8; and Cs6[Ga2O6] a = 7.26, b = 12.1, c = 7.68 Å, ß = 105°, Z = 4, space-group P21/a. 相似文献
4.
Thio- and Selenomercurates(II). K6[HgS4], K6[HgSe4], Rb6[HgS4] and Rb6[HgSe4] We prepared by annealing intimate mixture of pure samples of K2S, K2Se, Rb2S, and Rb2Se with HgS or HgSe [360–380°C, 7d, Duran-glass-seal with Argon] with hexagonal Na6ZnO4 isotypic new mercurates: K6[HgS4] [bright citronic yellow a = 9.985, c = 7.652 Å], K6[HgSe4] [light orange yellow a = 10.36, c = 7.883 Å], Rb6[HgS4] [bright yellow a = 10.34, c = 7.942 Å], Rb6[HgSe4] [orange-red a = 10.72, c = 8.192 Å]. The crystal structure of K6 Hgs4 is elucidated by using diffractometer data of single crystals: P63mc, C46v, it is R = 6.6% for 304 reflexes [h k o–h k 4, anisotropic refinement MoKα]; for position and parameters see text drö = 2.835, dpyk = 2.99 g · cm?3. The Madelung Part of Lattice Energy, MAPLE, and Effective Coordination Numbers, ECoN, are calculated and discussed. 相似文献
5.
Arno Lindemann Jrn Küper Christoph Jansen Joachim Kuchinke Christian Kster Adrienne Hammerschmidt Matthias Dch Timo Pruß Bernt Krebs 《无机化学与普通化学杂志》2001,627(3):419-425
The perseleno‐selenoborates Rb2B2Se7 and Cs3B3Se10 were prepared from the metal selenides, amorphous boron and selenium, the thallium perseleno‐selenoborates Tl2B2Se7 and Tl3B3Se10 directly from the elements in evacuated carbon coated silica tubes by solid state reactions at temperatures between 920 K and 950 K. All structures were refined from single crystal X‐ray diffraction data. The isotypic perseleno‐selenoborates Rb2B2Se7 and Tl2B2Se7 crystallize in the monoclinic space group I 2/a (No. 15) with lattice parameters a = 12.414(3) Å, b = 7.314(2) Å, c = 14.092(3) Å, β = 107.30(3)°, and Z = 4 for Rb2B2Se7 and a = 11.878(2) Å, b = 7.091(2) Å, c = 13.998(3) Å, β = 108.37(3)° with Z = 4 for Tl2B2Se7. The isotypic perseleno‐selenoborates Cs3B3Se10 and Tl3B3Se10 crystallize in the triclinic space group P1 (Cs3B3Se10: a = 7.583(2) Å, b = 8.464(2) Å, c = 15.276(3) Å, α = 107.03(3)°, β = 89.29(3)°, γ = 101.19(3)°, Z = 2, (non‐conventional setting); Tl3B3Se10: a = 7.099(2) Å, b = 8.072(2) Å, c = 14.545(3) Å, α = 105.24(3)°, β = 95.82(3)°, γ = 92.79(3)°, and Z = 2). All crystal structures contain polymeric anionic chains of composition ([B2Se7]2–)n or ([B3Se10]3–)n formed by spirocyclically fused non‐planar five‐membered B2Se3 rings and six‐membered B2Se4 rings in a molar ratio of 1 : 1 or 2 : 1, respectively. All boron atoms have tetrahedral coordination with corner‐sharing BSe4 tetrahedra additionally connected via Se–Se bridges. The cations are situated between three polymeric anionic chains leading to a nine‐fold coordination of the rubidium and thallium cations by selenium in M2B2Se7 (M = Rb, Tl). Coordination numbers of Cs+ (Tl+) in Cs3B3Se10 (Tl3B3Se10) are 12(11) and 11(9). 相似文献
6.
The compound [Co(En)3]2[Hg2(H2O)Cl6]Cl4 (I, En is ethylenediamine) has been synthesized and studied by X-ray diffraction. The crystals of I (a = 21.8745(14) Å, b = 10.6008(6) Å, c=15.4465(12) Å, space group Pna21) consist of tris(ethylenediamine)cobalt(III) complexes (the unit cell contains two [Co(En)3]3+ cations of opposite chirality). [Hg2(H2O)Cl6]2? anions, and isolated chloride ions. The complex anion consists of the tetrahedral [HgCl4]2? group (Hg-Cl, 2.44–2.56 Å) and the hydrated molecule [Hg(H2O)Cl2] (Hg-Cl, 2.301 and 2.308 Å; Hg-O, 2.788 Å) combined by weak Hg-Cl interactions (2.915 and 3.220 Å). 相似文献
7.
New compounds of the general formula A4[Nb6Cl12(NCS)6](H2O)4 (A = K, Rb, NH4) were synthesized from Nb6Cl14 and ASCN in aqueous solutions. X-ray structure refinements were performed on single-crystal data of the three compounds. They are isotypic and crystallize with the space group P1 (Z = 1) and the lattice parameters: a = 877.9(3) pm, b = 1176.6(3) pm, c = 1187.0(3) pm, α = 114.29(1)°, β = 98.96(2)°, γ = 100.91(2)° for K4[Nb6Cl12(NCS)6](H2O)4 ( 1 ); a = 887.6(3) pm, b = 1184.0(4) pm, c = 1195.4(4) pm, α = 114.95(2)°, β = 98.84(2)°, γ = 101.31(2)° for Rb4[Nb6Cl12(NCS)6](H2O)4 ( 2 ) and a = 886.0(4) pm, b = 1181.1(6) pm, c = 1183.9(6) pm, α = 114.49(2)°, β = 99.48(3)°, γ = 101.53(1)° for (NH4)4[Nb6Cl12(NCS)6](H2O)4 ( 3 ). Each centrosymmetric [Nb6Cl12(NCS)6]4? ion of the isotypic compounds contains six terminal thiocyanate groups being bound to the corners of the octahedral niobium cluster through the nitrogen atoms (dNb? N = 221.5(6)–224.3(6) pm, bond angles Nb? N? C 168.6(5)–176.4(6)°). The [Nb6Cl12(NCS)6]4? ions are linked via A? S and A? Cl interactions with the A cations. Half of the cations occur to be disordered along two crystallographic sites. 相似文献
8.
New Metal Oxides with Doubles of Tetrahedra as Building Units: Rb6[Tl2O6] and Cs6[In2O6] We prepared the hitherto unknown Rb6[Tl2O6] and Cs6[In2O6] by heating mixtures of Tl2O3 and RbO0.60 (Rb:Tl = 3.5:1) as well as In2O3 and CsO0.53 (Cs:In = 3.5:1) as single crystals [closed Ag-cylinder, 650°C, 14 d]. The single crystals of Rb6[Tl2O6] are yellow, those of Cs6[In2O6] pale yellow, all transparent and rude. The new type of structure was elucidated by 4-circle-diffractometer (PW 1100) data. Rb6[Tl2O6]: P21/a; a = 1145,7(3), b = 713,3(1), c = 783,9(2) pm, β = 93,73° (2), Z = 2; Ag–Kα, 2100 out of 2531 I0(hkl), R = 9,6% and Rw = 8,9%. Cs6[In2O6]: P21/a; a = 1178,5(4), b = 730,7(2), c = 816,3(2) pm, β = 95,38° (3), Z = 2; Mo–Kα, 1584 out of 2032 I0(hkl), R = 9,25%, and Rw = 8,44%. The Madelung Part of Lattice Energy, MAPLE, is calculated and discussed. 相似文献
9.
Chloro- and Polyselenoselenates(II): Synthesis, Structure, and Properties of [Ph3(C2H4OH)P]2[SeCl4] · MeCN, [Ph4P]2[Se2Cl6], and [Ph4P]2[Se(Se5)2] By symproportionation of elemental selenium and SeCl4 in polar protic solvents the novel chloroselenates(+II), [SeCl4]2? and [Se2Cl6]2?, could be stabilized; they were crystallized with voluminous organic cations. They were characterized from complete X-ray structure analysis. Yellow-orange [Ph3(C2H4OH)P]2[SeCl4] · MeCN (space group P1 , a = 10.535(4), b = 12.204(5), c = 16.845(6) Å, α = 77.09(3)°, β = 76.40(3)°, γ = 82.75(3)° at 140 K) contains in its crystal structure monomeric [SeCl4]2? anions with square-planar coordination of Se(+II). The mean Se? Cl bond length is 2.441 Å. In yellow [Ph4P]2[Se2Cl6] (space group P1 , a = 10.269(3), b = 10.836(4), c = 10.872(3) Å, α = 80.26(3)°, β = 79.84(2)°, γ = 72.21(3)° at 140 K) a dinuclear centrosymmetric [Se2Cl6]2? anion, also with square-planar coordinated Se(+II), is observed. The average terminal and bridging Se? Cl bond distances are 2.273 and 2.680 Å, respectively. From redox reactions of elemental Se with boranate/thiolate in ethanol/DMF the bis(pentaselenido)selenate(+II) anion [Se(Se5)2]2? was prepared as a novel type of a mixed-valent chalcogenide. In dark-red-brown [Ph4P]2[Se(Se5)2] (space group P21/n, a = 12.748(4), b = 14.659(5), c = 14.036(5) Å, β = 108.53(3)° at 140 K) centrosymmetric molecular [Se(Se5)2]2? anions with square-planar coordination of the central Se(+II) by two bidentate pentaselenide ligands is observed (mean Se? Se bond lengths: 2.658 Å at Se(+II), 2.322 Å in [Se5]2?). The resulting six-membered chelate rings with chair conformation are spirocyclically linked through the central Se(+II). The vibrational spectra of the new anions are reported. 相似文献
10.
New Oxozineates of Alkali Metals: Rb2[ZnO2] and Cs2[ZnO2] Colorless single crystals of the hitherto unknown Rb2[ZnO2] (a = 9.558, b = 6.335, c = 15.91 Å, β = 118.6°, z = 8, dpyk = 4.11, drö = 4.21 g · cm?3) and Cs2[ZnO2] (a = 9.851, b = 6.619, c = 16.26 Å, β = 116.8°) have been prepared, which crystallize monoclinic, P21/c – D. (For parameters see text.) Unexpected there are “isolated” groups [Zn4O8]. Half of the Zn atoms exhibit the unusual coordination number 3 towards O2?. The Madelung Part of Lattice Energy, MAPLE, and the Effective Coordination Number, ECoN, the latter by means of Mean Fictive Ionic Radii, MEFIR, are calculated and discussed. 相似文献
11.
Synthesis and Crystal Structures of [P(C6H5)4][1-(NH3)B10H9] and Cs[(NH3)B12H11] · 2CH3OH The reduction of [1-(NO2)B10H9]2? with aluminum in alkaline solution yields [1-(NH3)B10H9]? and by treatment of [B12H12]2? with hydroxylamine-O-sulfonic acid [(NH3)B12H11]? is formed. The crystal structures of [P(C6H5)4][1-(NH3)B10H9] (triclinic, space group P1 , a = 7.491(2), b = 13.341(2), c = 14.235(1) Å, α = 68.127(9), β = 81.85(2), γ = 86.860(3)°, Z = 2) and Cs[(NH3)B12H11] · 2CH3OH (monoclinic, space group P21/n, a = 14.570(2), b = 7.796(1), c = 15.076(2) Å, β = 111.801(8)°, Z = 4) reveal for both compounds the bonding of an ammine substituent to the cluster anion. 相似文献
12.
H. Imoto N. G. Naumov A. V. Virovets T. Saito V. E. Fedorov 《Journal of Structural Chemistry》1998,39(5):720-727
Crystal structures of Cs4[Re6Te8(CN)6]·2H2O (1) and Ba2[Re6Te8(CN)6]· 12H2O (2) are determined. Crystals 1 are orthorhombic, a = 14,282(1), b = 12.910(1), c = 18.040(1) Å, Vcell = 3326.3(8) Å3, space group Pbcn, Z = 4, dcalc = 5.715 g/cm3, R(F) = 0.0482 for 3193 Fhkl > 4σ(F). Crystals 2 are triclinic, a = 9.671(3), b = 9.697(4), c = 11.039(4) Å, α = 89.86(3), β = 72.34(3), γ = 82.46(3)°, Vcell = 977.2(6) Å3, space group P1, Z = 1, dcalc = 4.733 g/cm3, R(F) = 0.0490 for 3226 Fhkl > 4σ(F). In both structures, the [Re6Te8(CN)6]4? anions form a distorted primitive cubic packing with distances between the centers 9.02-9.63 Å in 1 and 9.70-11.04 Å in 2. The Cs+ cations in 1 lie near the face centers of the cubes formed by the onions. In 2, cation pairs (Ba2+)2 bonded to two solvate water molecules are formed; the pairs lie at the centers of the anion cubes. In structures 1 and 2, there are shortened contacts between the tellurium atoms belonging to the neighboring anions (3.75-4.09 and 3.95-4.22 Å, respectively). 相似文献
13.
On TiF3 and Hexafluorotitanates(III): Cs2K[TiF6] and Rb2K[TiF6], with a remark on Rb3[TiF6] By “redox-reaction with the wall” according to A2B[CuF6] + Ti = A2B[TiF6] + Cu we obtained for the first time single crystals of the Hexafluorotitanates(III). The violett irregular single crystals of Cs2K[TiF6] (a = 9.115 Å) and Rb2K[TiF6] (a = 8.910 Å) crystalise in accordance with the single-crystal studies as supposed in spcgrp. O-Fm3m No. 225. Dark blue crystals of TiF3 crystalises in the VF3-Typ. Parameters see text. TiF3 (3.9–251.3 K) and Rb3[TiF6] (3.8–251.3 K) have been measured magnetically. The madelung part of lattice energy, MAPLE, and the effective coordination number, ECoN, via the mean fictive ionic radii, MEFIR, are calculated and discussed. 相似文献
14.
Molybdenum(II) Halide Clusters with two Alcoholate Ligands: Syntheses and Crystal Structures of (C18H36N2O6Na)2[Mo6Cl12(OCH3)2] and (C18H36N2O6Na)2[Mo6Cl12(OC15H11)2] · 2C4H6O3 . Reaction of Mo6Cl12 with two equivalents of sodium methoxide in the presence of 2,2,2-crypt yields (C18H36N2O6Na)2[Mo6Cl12(OCH3)2] ( 1 ), which can be converted to (C18H36N2O6Na)2[Mo6Cl12(OC15H11)2] · 2C4H6O3 ( 2 ) by metathesis with 9-Anthracenemethanole in propylene carbonate. As confirmed by X-ray single crystal structure determination ( 1 : C2/m, a=25.513(8) Å, b=13.001(3) Å, c=10.128(3) Å, β=100.204(12)°; : C2/c, a=15.580(5) Å, b=22.337(5) Å, c=27.143(8) Å, β=98.756(10)°) the compounds contain anionic cluster units [Mo6ClCl(ORa)2]2? with two alcoholate ligands in terminal trans positions ( 1 : d(Mo—Mo) 2.597(2) Å to 2.610(2) Å, d(Mo—Cli) 2.471(3) Å to 2.493(4) Å, d(Mo—Cla) 2.417(8) Å and 2.427(8) Å, d(Mo—O) 2.006(13) Å; 2 : d(Mo—Mo) 2.599(3) Å to 2.628(3), d(Mo—Cli) 2.468(8) Å to 2.506(7) Å, d(Mo—Cla) 2.444(8) Å and 2.445(7) Å, d(Mo—O) 2.012(19) Å). 相似文献
15.
Synthesis and Structures of the Selenolato-Bridged Mercury Clusters [Hg6(SePh)12(P t Bu3)2] and (HP t Bu3)2[Hg6(SePh)14] The reaction of HgCl2 with PtBu3 and PhSeSiMe3 yields [Hg6(SePh)12(PtBu3)2] ( 1 ) and (HPtBu3)2[Hg6(SePh)14] ( 2 ). X-ray structural analysis of the compounds shows them to have similar Hg–Se cages with distorted tetrahedral coordination around mercury. The cages are built up from edge- and vertex-sharing distorted tetrahedra. 相似文献
16.
Contributions on Crystal Structures and Thermal Behaviour of Anhydrous Phosphates. XXIII. Preparation, Crystal Structure, and Thermal Behaviour of the Mercury(I) Phosphates α-(Hg2)3(PO4)2, β-(Hg2)3(PO4)2, and (Hg2)2P2O7 Light-yellow single crystals of (Hg2)2P2O7 have been obtained via chemical vapour transport in a temperature gradient (500 °C → 450 °C, 23 d) using Hg2Cl2 as transport agent. Characteristic feature of the crystal structure (P2/n, Z = 2, a = 9,186(1), b = 4,902(1), c = 9,484(1) Å, β = 98,82(2)°, 1228 independent of 5004 reflections, R(F) = 0,066 for 61 variables, 7 atoms in the asymmetric unit) are Hg22+-units with d(Hg1–Hg1) = 2,508 Å and d(Hg2–Hg2) = 2,519 Å. The dumbbells Hg22+ are coordinated by oxygen, thus forming polyhedra [(Hg12)O4] and [(Hg22)O6]. These polyhedra share some oxygen atoms. In addition they are linked by the diphosphate anion P2O74– (ecliptic conformation; ∠(P,O,P) = 129°) to built up the 3-dimensional structure. Under hydrothermal conditions (T = 400 °C) orange single crystals of the mercury(I) orthophosphates α-(Hg2)3(PO4)2 and β-(Hg2)3(PO4)2 have been obtained from (Hg2)2P2O7 and H3PO4 (c = 1%). The crystal structures of both modifications have been refined from X-ray single crystal data [α-form (β-form): P21/c (P21/n), Z = 2 (2), a = 8,576(3) (7,869(3)), b = 4,956(1) (8,059(3)), c = 15,436(3) (9,217(4)) Å, β = 128,16(3) (108,76(4))°, 1218 (1602) independent reflections of 4339 (6358) reflections, R(F) = 0,039 (0,048) for 74 (74) variables, 8 (8) atoms in the asymmetric unit]. In the structure of α-(Hg2)3(PO4)2 three crystallographically independent mercury atoms, located in two independent dumbbells, are coordinated by three oxygen atoms each. Thus, [(Hg2)O6] dimers with a strongly distorted tetrahedral coordination of all mercury atoms are formed. Such dimers are present besides [(Hg2)O5]-polyhedra in the less dense crystal structure of β-(Hg2)3(PO4)2 (d(Hg–Hg) = 2,518 Å). The mercury(I) phosphates are thermally labile and disproportionate between 200 °C (β-(Hg2)3(PO4)2) and 480 °C (α-(Hg2)3(PO4)2) to elemental mercury and the corresponding mercury(II) phosphate. 相似文献
17.
Crystal Structure of Tetraphenylphosphonium Monothiocyanatohydro-closo-Decaborate, [P(C6H5)4]2[2-(SCN)B10H9] · CH3CN The X-ray structure determination of [P(C6H5)4]2[2-(SCN)B10H9] · CH3CN (monoclinic, space group P21/n, a = 10.6040(10), b = 13.8880(9), c = 33.888(3) Å, β = 94.095(8)°, Z = 4) reveals the S coordination of the SCN substituent with a B? S distance of 1.913(6) Å and a B? S? C angle of 105.3(3)°. The SCN group is nearly linear (178.2(7)°). 相似文献
18.
Mehmet Somer Wilder Carrillo-Cabrera Eva Maria Peters Karl Peters Hans Georg von Schnering 《无机化学与普通化学杂志》1998,624(11):1915-1921
Tetrarubidiumnonagermanid(4–)-ethylendiamin, Rb4[Ge9][en] Orange-farbene Kristalle von Rb4[Ge9][en] erhält man nach der Austauschreaktion einer Lösung von ,NaGe2.25‘ (precursor) in Ethylendiamin (en) mit festem RbI bei 360 K und nachfolgender langsamer Abkühlung. Die Verbindung ist äußerst empfindlich gegen Oxidation und Hydrolyse. Der thermische Abbau im dynamischen Vakuum beginnt mit der vollständigen Abgabe von en bei 350 K. Es folgt die Sublimation von Rubidium in vier weiteren Stufen (Rb8Ge25, Rb8Ge44, RbxGe136 mit x È 16, Ge). Das Ramanspektrum zeigt die charakteristischen Banden des Anions [Ge9]4– bei 151, 163, 185 und 222 cm–1. Rb4[Ge9][en] kristallisiert in einem neuen Strukturtyp (Raumgruppe P21/m; a = 15.353 Å, b = 16.434 Å, c = 15.539 Å, β = 113.75°; Z = 6; Pearsonsymbol mP198-40), der als hierarchische Variante der Strukturen von Al4YbMo2 und CrB4 (hierarchische Basistypen, „initiators”︁) beschrieben werden kann, indem Atome partiell durch Aggregate ersetzt werden: B4[□][Cr] ≙ Al4[Yb][Mo]2 ≙ Rb4[Ge9][en]1–2. Drei kristallographisch unabhängige [Ge9]4–-Cluster sind in ein vierbindiges 465-Netz aus Rb-Atomen eingebettet, ein Netzwerk kondensierter Tetraasterane. Die Cluster sind verzerrte überkappte tetragonale Antiprismen mit D1(Ge–Ge) = 2.57 Å (16 Ç ) und D2(Ge–Ge) = 2.84 Å (4 Ç ). Die Atome der Cluster mit D1 und D2 liegen auf der Oberfläche eines Rotationsellipsoids (a = b = 2.136 Å, c = 2.431 Å). Die en-Moleküle befinden sich in offenen Kanälen entlang [1¯ 0 1]. Die Koordinationen [Ge9]Rb12/4 und Rb [Ge9]4/12 en2/8 zeigen, daß beim ersten Schritt der Solvatisierung Kationen und Clusteranionen nicht voneinander getrennt werden. 相似文献
19.
Crystal Structure, Vibrational Spectra, and Normal Coordinate Analysis of ( n ‐Bu4N)2[Os(NCS)6] and ( n ‐Bu4N)3[Os(NCS)6] By tempering the solid mixture of the linkage isomers (n‐Bu4N)3[Os(NCS)n(SCN)6–n] n = 0–5 for a longer time at temperatures increasing from 60 to 140 °C the homoleptic (n‐Bu4N)3[Os(NCS)6] is formed, which on oxidation with (NH4)2[Ce(NO3)6] in acetone yields the corresponding OsIV complex (n‐Bu4N)2[Os(NCS)6]. X‐ray structure determinations on single crystals of (n‐Bu4N)2[Os(NCS)6] (1) (triclinic, space group P 1, a = 12.596(5), b = 12.666(5), c = 16.026(5) Å, α = 88.063(5), β = 80.439(5), γ = 88.637(5)°, Z = 2) and (n‐Bu4N)3[Os(NCS)6] ( 2 ) (cubic, space group Pa 3, a = 24.349(4) Å, Z = 8) have been performed. The nearly linear thiocyanate groups are coordinated with Os–N–C angles of 172.3–177.7°. Based on the molecular parameters of the X‐ray determinations the IR and Raman spectra are assigned by normal coordinate analysis. The valence force constant fd(OsN) is 2.3 ( 1 ) and 2.10 mdyn/Å ( 2 ). 相似文献
20.
Halomercurates: Syntheses and Crystal Structures of [Cu(en)2][Hg2Cl6], [Cu(en)2][Hg2Br6], and [Cu(en)2][HgBr4] Crystals of [Cu(en)2][Hg2Cl6] ( 1 ) have been obtained by layering a solution of Hg(NO3)2 and NaCl with a solution of [Cu(en)2]SO4. An analogous procedure, using NaBr instead of NaCl, gave crystals of [Cu(en)2][HgBr4] ( 3 ). Crystals of [Cu(en)2][Hg2Br6] ( 2 ) were obtained by gel crystallization using the same starting materials as for 3 . The complexes show very low solubility. The dinuclear anions of 1 consist of two nearly planar HgCl3 units related by a center of symmetry. In 2 infinite anionic chains are present, made up of parallel HgBr3 units. These units are packed in such a way as to produce a trigonal bipyramidal configuration around the Hg atoms. 3 contains mononuclear deformed tetrahedral [HgBr4]2– anions. In all three complexes the packing of the ions is such that halogen atoms of halomercurate anions complete a tetragonal bipyramidal coordination at Cu. The resulting Cu–Halogen distances are 2.924 Å for 1 , 3.036 Å for 2 and 3.085 and 3.119 Å for 3 . 1 : Space group P 1, Z = 1, lattice constants at 20 °C: a = 7.000(2), b = 7.526(2), c = 8.239(2) Å; α = 88.39(2), β = 86.06(2), γ = 86.10(3)°; R1 = 0.040. 2 : Space group P21/c, Z = 2, lattice constants at –50 °C: a = 7.185(1), b = 16.338(2), c = 7.814(1) Å; β = 94.88(2)°; R1 = 0.033. 3 : Space group P21/n, Z = 4, lattice constants at 20 °C: a = 8.055(3), b = 13.101(3), c = 13.814(3) Å; β = 91.24(3)°; R1 = 0.092. 相似文献