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1.
A clathrate compound [MnPy4(NO3)2]·2Py was synthesized and studied by single-crystal X-ray diffraction analysis (KM-4 diffractometer, CuKα,ω/2? scan mode,? max=78°). The unit cell is base-centered orthorhombic, space group Ccca, a=12.097(4), b=15.197(4), c=17.213(4) Å, V=3164(2) Å3, Z=4, R=0.072, for 632 reflections and 107 parameters in the least-squares analysis. The host molecule has 222 symmetry. Two monodentate nitrato groups and four pyridine ligands are coordinated to Mn(II) along the symmetry axes (the former via O). The pyridine guest molecules lie in the cavities of the crystal framework. For [MnPy3(NO3)2)], only unit cell parameters were determined: a=12.467(5), b=9.514(2), c=16.383(5) Å,β=108.93(4), V=1838(1) Å3 space group C2/c or Cc (according to extinctions). The pyridine-manganese nitrate system is shown to be analogous to the previously investigated Co, Ni, Cu, Zn, and Cd systems. 相似文献
2.
A. G. Mirochnik B. V. Bukvetskii P. A. Zhikhareva N. V. Polyakova V. E. Karasev 《Russian Journal of Inorganic Chemistry》2006,51(5):737-742
The crystal structure of the [Tb(BTFA)2(NO3)(TPPO)2] complex (TPPO is triphenylphosphine oxide, BTFA is benzoyltrifluoracetone), which exhibits strong triboluminescence, has been established by X-ray crystallography. The crystals are triclinic: a = 11.668(3) Å, b = 11.700(3) Å, c = 12.512(3) Å, α = 65.161(4°), β = 79.120(4)°, γ = 61.860(4)°, space group P1, Z = 1. The central terbium(III) atom coordinates two oxygen atoms from two triphenylphosphine oxide molecules (Tb-O, 2.264(3) and 2.273(3) Å), two oxygen atoms from the nitrate group (Tb-O, 2.460(3) and 2.476(3) Å), and four oxygen atoms from two benzoyltrifluoroacetonate groups (Tb-O, 2.329(3), 2.399(3), 2.351(3), and 2.367(3) Å). The coordination polyhedron of the Tb(III) atom is a distorted dodecahedron. The photoluminescence and triboluminescence spectra of the [Tb(BTFA)2(NO3)(TPPO)2] complex are identical and caused by the f-f luminescence of Tb3+. 相似文献
3.
A coordination polymer, catena((μ2-4,4,10,10-tetramethyl-1,3,7,9-tetraazaspiro[5.5]undecane- 2,8-dione-O,O')-aquadinitratocadmium(II) {[Cd(C11H20N4O2)(H2O)(NO3)2]} n } (I), has been prepared for the first time from cadmium(II) nitrate and the bicyclic bisurea 4,4,10,10-tetramethyl-1,3,7,9-tetraazaspiro[5.5]undecane-2,8-dione (TTSU). Its molecular structure has been determined (CIF file CCDC no. 903387). Triclinic crystals: space group P1?, a = 8.9967(4) Å, b = 9.6011(4) Å, c = 12.5131(7) Å, α = 76.307(4)°, β = 73.465(5)°, γ = 63.310(5)°, V = 918.26(8) Å3, ρcalc = 1.789 g/cm3, Z = 2. The Rietveld refinement was carried out at 293 K to confirm the single-phase constitution of the obtained powder sample of I: a = 8.9972(4) Å, b = 9.6104(4) Å, c = 12.5203(4) Å, α = 76.373(3)°, β = 73.485(3)°, γ = 73.485(3)°, V = 919.80(6) Å3. A number of lines not corresponding to the main phase and not identified from PDF-2 database are observed on the powder X-ray diffraction pattern. The Rietveld refinement showed that the sample contains 91.4 wt % of the main compound I and 8.6 wt % of the TTSU nitrate admixture. The cadmium atom is coordinated by the O(1) and O(1)i atoms of two molecules of the organic ligand (L) generated by the symmetry operation (i1–x,–y,–z), the O(2)ii atom of the third ligand L molecule bound with the supporting one with the symmetry operation (ii–x,–y,–z), a water molecule, and a bidentate and a monodentate nitrate anions. The coordination number of the cadmium atom is 7, the coordination polyhedron is a distorted pentagonal bipyramid. The Cd···Cd distance is 4.0208 (3) Å. 相似文献
4.
Yu. V. Kokunov Yu. E. Gorbunova V. V. Kovalev S. A. Kozyukhin 《Russian Journal of Inorganic Chemistry》2013,58(10):1187-1192
The coordination compounds [CoL2Cl2] (I) and [CdL2(H2O)2(NO3)2] (II) have been synthesized by the reaction of CoCl2 · 6H2O and Cd(NO3)2 · 4H2O with L = 2-amino-4-methylpyrimidine (Ampym, C5H7N3), and their structures have been solved. The crystals of complex I are triclinic, space group $P\bar 1$ , a = 5.627(1) Å, b = 11.191(1) Å, c = 12.445(1) Å, α = 81.00(1)°, β = 77.21(1)°, γ = 76.18(1)°, V = 737.7(2) Å3, ρcalcd = 1.567 g/cm3, Z = 2. The crystals of complex II are monoclinic, space group P21/c, a = 10.390(1) Å, b = 11.982(1) Å, c = 7.624(1) Å, β = 102.61(1)°, V = 926.1(2) Å3, ρcalcd = 1.760 g/cm3, Z = 2. Discrete [CoL2Cl2] moieties are realized in the structure of complex I. The cobalt atom is tetrahedrally coordinated to the two nitrogen atoms of crystallographically nonequivalent ligands L and two chlorine atoms (Co(1)-Navg, 2.051(4)Å; Co(1)-Cl(1), 2.241(1) Å; Co(1)-Cl(2), 2.263 Å; bond angles at the cobalt atom lie within a range of 102.1°–118.6°). The complexes are linked into supramolecular zigzag chains by N-H...N(Cl) hydrogen bonds. In the structure of complex II, the Cd2+ ion (at the inversion center) is coordinated in pairs to the nitrogen atoms of ligand L and the O(NO3) and O(H2O) oxygen atoms. The coordination of the Cd2+ ion is distorted octahedral (Cd(1)-N(1), 2.341Å; Cd(1)-O(1), 2.340(4) Å; Cd(1)-O(4), 2.327(3) Å; bond angles at the cadmium atom lie within a range of 79.1°–100.9°). N-H...N hydrogen bonds link the complexes into supramolecular chains. These chains are linked into a supramolecular framework by the O-H...O hydrogen bonds between water molecules and NO3 groups. 相似文献
5.
Cd(NO3)2 undergoes a phase transition at 160°C. The high temperature form is cubic and isomorphic with M(NO3)2 (M = Ba, Ca, Sr, Pb). The crystal structure of the low temperature phase has been solved by X-ray diffraction at 20°C, using 774 independent reflections collected with a 4-circle diffractometer. The dimensions of the orthorhombic unit cell are: Å, b = 15.3692 (35) Å, Z = 8, space group Pca21. The structure has been refined to the final weighted R = 0.044. The cadmium atoms are nearly in a face-centered arrangement. Each cadmium is octahedrally surrounded by six oxygen, the CdO distances varying from 2.34 to 2.46 Å. Each nitrate group belongs through its three oxygens to three different octahedra. The structural change cubic Cd(NO3)2 → orthorhombic Cd(NO3)2 is characterized by a small rotation of NO3 groups in their plane; the face-centered array of cadmium atoms is only slightly modified. The coordination of cadmium atoms changes from 12 to 6, and the approximate doubling of parameter (b) as well as the difference of symmetry can be explained by two different directions of rotation of the NO3 groups situated in the same plane. 相似文献
6.
Compounds [Rh(NH3)5(NO2)](NO3)2·H2O (I) with a = 7.6230(3) Å, b = 7.6230(3) Å, c = 10.3584(4) Å, space group I-42m, Z = 2, d calc = 2.026 g/cm3, V = 601.93(4) Å3, Rh-NH3 eq = 2.074 Å, Rh-NH3 ax (NO2) = 2.048 Å; [Rh(NH3)5(NO2)][Pd(NO2)4] (II) with a = 8.095(3) Å, b = 22.422(8) Å, c = 7.887(3) Å, β = 98.559(17)°, space group Cc, Z = 4, d calc = 2.461 g/cm3, V = 1415.6(9) Å3, Rh-NH3 eq = 2.069 Å, Rh-NH3 ax = 2.090 Å, Rh-NO2 = 2.002 Å; K2[Rh(NH3)(NO2)5]·H2O (III) with a = 7.5177(5) Å, b = 20.9856(15) Å, c = 7.7017(5) Å, space group Cmc21, Z = 4, d calc = 2.439 g/cm3, V = 1215.05(14) Å3, Rh-NH3 ax (NO2) = 2.094 Å, Rh-NO2 eq = 2.030 Å are synthesized and studied using single crystal X-ray diffraction. 相似文献
7.
S. P. Khranenko I. A. Baidina S. A. Gromilov A. V. Belyaev 《Journal of Structural Chemistry》2005,46(6):1060-1065
Powder and single crystal X-ray diffraction studies have been performed for anhydrous nitrate complexes Rb2[Pd(NO3)4] (I) and Cs2[Pd(NO3)4] (II). Crystal data for I: a = 7.843(1) Å, b = 7.970(1) Å, c = 9.725(1) Å; β = 100.39(1)°, V = 597.9(1) Å 3, space group P21/c, Z = 2, d calc = 2.918 g/cm3; for II: a = 10.309(2) Å, b = 10.426(2) Å, c = 11.839(2) Å; β = 108.17(3)°, V = 1209.0(4) Å3, space group P21/c, Z = 4, d calc = 3.408 g/cm3. The structures are formed by isolated [Pd(NO3)4]2? complex anions and alkali metal cations. The plane-square environment of the Pd atom is formed from the oxygen atoms of the monodentate nitrate groups. The geometrical characteristics of the complex anions are analyzed. Compound II has a short contact Pd...Cs 3.252 Å. 相似文献
8.
Yu. V. Kokunov Yu. E. Gorbunova V. V. Kovalev 《Russian Journal of Inorganic Chemistry》2011,56(6):856-860
Complex [Ni(NO3)2(3,5-lutidine)3] (3,5-lutidine, 3,5-Lut-C7H9N) was synthesized, and its crystal structure was determined. Complex crystals are monoclinic: space group Cc, a = 14.445(1) Å, b = 10.024(1) Å, c = 17.607(1) Å, β = 108.96(1)°, V = 2411(1) Å3, ρcalcd = 2.389 g/cm3, Z = 4. The structure is built of discrete neutral complexes [Ni(3,5-Lut)3(NO3)2]. The coordination sphere of Ni2+ ions is a disordered octahedron, which consists of three crystallographically nonequivalent lutidine ligands (Ni-N, 2.059–2.124 Å) and two oxygen ions of the two nitrate ions (Ni-O, 2.047–2.258 Å). 相似文献
9.
《Journal of Coordination Chemistry》2012,65(3):390-399
Coordination polymers, {[Cd(2-mBIM)3](ClO4)2} n (1) and [Cd(BIM)2(NO3)2] n (2), have been prepared from the reaction of bis(2-methylimidazol-1-yl)methane(2-mBIM) with Cd(ClO4)2 and bis(imidazol-1-yl)methane (BIM) with Cd(NO3)2 in ethanol and water, respectively. Their structures were characterized by single crystal X-ray diffraction and IR spectroscopy. Compound 1 crystallizes in the rhombohedral space group R-3c with a = b = 12.3617(5) Å, c = 38.896(3) Å, γ = 120°, V = 5147.5(5) Å3, z = 6. The CdII occupies a crystallographic inversion center and is coordinated by six N atoms from six distinct 2-mBIM ligands to form a slightly distorted octahedral geometry. Each 2-mBIM is coordinated to two CdII cations, linking alternatively four CdII cations, resulting in a 32-membered M4L4 macrometallacycle. Compound 2 crystallizes in the monoclinic space group C2/m with a = 14.400(3) Å, b = 9.3894(18) Å, c = 8.6926(17) Å, β = 123.499(2)°, V = 980.1(3) Å3, z = 2. The Cd coordinates to four nitrogen atoms from four different BIM and two nitrates to form a slightly distorted octahedral geometry. The BIM ligands bridge to form a 1-D infinite double-bridged chain structure with 16-membered M2L2 macrometallacyclic structural units. 相似文献
10.
É. B. Miminoshvili K. É. Miminoshvili S. R. Zazashvili L. A. Beridze 《Journal of Structural Chemistry》2006,47(6):1188-1192
Synthesis of [Cu(m-HBH)2(OH2)2](NO3)2·2H2O, where m-HBH = C7H8O2N2 (3-hydroxybenzoylhydrazine), is described. The structure of the compound was studied by X-ray phase analysis and IR spectroscopy; crystal data are a = 57.415(6) Å, b = 19.760(2) Å, c = 7.586(2) Å; Fdd 2, Z = 16, R(F) = 0.053. The compound consists of [Cu(m-HBH)2(OH2)2]2+ complex cations, NO 3 ? anions, and two water molecules. The similarity between the IR spectra of Cu(m-HBH)2(NO3)2·nH2O and Co(m-HBH)2(NO3)2·5H2O, element analysis data, and crystal data obtained at the first stage of X-ray analysis show that the structures and compositions of these compounds are identical relative to the type of surroundings of the central atom. In contrast to the cobalt compound [Co(m-HBH)2(OH2)2](NO3)2·3H2O, in which the cobalt atom has a nearly regular octahedron as a coordination polyhedron, the copper(II) compound has a square bipyramid around the copper atom; c.n. is 6 = 4 + 2 (planar distances: 2.013(2) Å, 2.021(2) Å, 2.033(3) Å, 2.087(3) Å; axial distances: 2.367(3) Å, 2.374(3) Å) and lacks one crystallization water molecule. 相似文献
11.
《Comptes Rendus de l''Academie des Sciences Series IIB Mechanics Physics Astronomy》1998,1(7):417-420
The cobalt(II) complex of 3-methoxy 2-hydroxybenzaldehyde, L2Co(H2O)2 reacts with lanthanide nitrates to afford dinuclear complexes L2Co(H2O)2Ln(NO3)3. An X-ray diffraction study of L2Co(H2O)2Pr(NO3)3 has been performed. It crystallizes in the monoclinic space group P21/c, in a cell having the dimensions a = 9.4832(11) Å, b = 18.319(2) Å, c = 14.6226(13) Å and β = 106.121(12)° and Z = 4. The magnetic properties of L2Co(H2O)2Gd(NO3)3 revealed that a ferromagnetic interaction occurs between the Co2+ and Gd3+ ions. 相似文献
12.
A. A. Tripolskaya E. A. Mainicheva T. V. Mit'kina O. A. Geras'ko D. Yu. Naumov V. P. Fedin 《Russian Journal of Coordination Chemistry》2005,31(11):768-774
Slow evaporation of solutions of Sc and Eu nitrates with macrocyclic cavitand cucurbit[6]uril gives crystals of isostructural complexes [Sc(NO3)(H2O)4(C36H36N24O12)](NO3)2 ? 8.5H2O (space group Pna21, a = 32.0065(18) Å, b = 14.7904(8) Å, c = 11.5774(6) Å, V = 5480.6(5) Å3, Z = 4) and [Eu(NO3)(H2O)4(C36H36N24O12)](NO3)2 ? 6.75H2O (space group Pna21, a = 31.9525(17) Å, b = 14.7203(8) Å, c = 11.8592(6) Å, V = 5578.0(5) Å3, Z = 4). The metal to ligand ratio in these complexes is 1 : 1; the complexes are obtained at 0.025–0.1 mol/l concentrations of the metals in solutions. With higher lanthanide concentrations (0.7–1 mol/l), the 2 : 1 complex with cucurbit[6]uril is formed of the composition [{ Gd(NO3)(H2O)5}2(C36H36N24O12)](NO3)4 ? 6.5H2O (space group \(P\bar 1\), a = 13.3972(6) Å, b = 14.4994(5) Å, c = 18.3290(8) Å, α = 73.5610(10)°, β = 87.2590(10)°, γ = 87.5540(10)°, V = 3409.4(2) Å3, Z = 2) and isotypical complex [{Gd(NO3)(H2O)5}2{(C5H5N) ? (C36H36N24O12)}](NO3)4 ? 8H2O with a pyridine molecule inside the cucurbit[6]uril cavity (space group P21/n, a = 14.8263(6) Å, b = 13.3688(7) Å, c = 18.5970(9) Å, β = 107.5860(10)°, V = 3513.8(3) Å3, Z = 2). According to X-ray diffraction data, the metal atoms of the title complexes coordinate the O atoms in portals of cucurbit[6]uril molecules. 相似文献
13.
A. S. Antsyshkina G. G. Sadikov T. B. Kuvshinova V. M. Skorikov V. S. Sergienko 《Russian Journal of Inorganic Chemistry》2006,51(3):374-385
A novel compound, KBi(C6H4O7) · 3.5H2O (I), has been synthesized in the Bi(NO3)2-K3(HCit) system (HCit3? is an anion of citric acid C6H8O7) at a component ratio (n) of 8 in a water-glycerol mixture, and its crystal structure has been determined. The crystals are unstable in air. The crystals are triclinic: a = 7.462 Å, b = 10.064 Å, c = 17.582 Å, α = 100.27°, β = 99.31°, γ = 105.48°, V = 1221.2 Å3, Z = 2, space group $P\bar 1$ . In the structure of I, asymmetric binuclear fragments [Bi2(Cit4?)2(H2O)2]2? are linked through inversion centers into polymeric chain anions. Ions K+ and crystal water molecules are arranged in channels between the chains. The Bi(1)...Bi(2) distances in the binuclear fragment are 4.62 Å, and the Bi(1)...Bi(1) and Bi(2)...Bi(2) distances between bismuth atoms in the chain are 5.83 and 5.95 Å, respectively. The chains are linked through bridging oxygen atoms of the ligands Cit to form layers. In the centrosymmetric four-membered chelate ring Bi2O2 formed through Bi-O(Cit) bonds, the distances Bi(1)-Bi(1) are equal to 4.55 Å, and Bi(1)-O are 2.66 and 2.84 Å. The Bi-O bond lengths in I are in the range 2.12–3.16 Å. The Cit ligands act as hexadentate chelating/bridging ligands. 相似文献
14.
B. V. Bukvetskii A. G. Mirochnik P. A. Zhikhareva V. E. Karasev 《Journal of Structural Chemistry》2006,47(3):575-580
The crystal structure of [Eu(TTA)2(NO3)(TPPO)2] (I) (TTA = thenoyltrifluoroacetone, TPPO = triphenylphosphine oxide) possessing intense triboluminescence was established by X-ray crystallography. The crystals are triclinic, noncentrocymmetrical: a = 11.047(3) Å, b = 11.794(3) Å, c = 12.537(3) Å; α = 102.635 (4)°, β = 102.088(4)°,γ = 117.765(3)°; space group P1, Z = 1. The central Eu(III) atom coordinates two oxygen atoms of two TPPO molecules at distances of 2.271 Å and 2.282 Å, two oxygen atoms of the nitrate group at distances of 2.478 Å and 2.481 Å, four oxygen atoms of two TTA ions at distances of 2.365 Å, 2.381 Å, and 2.363 Å, 2.371 Å (coordination number is 8). The coordination polyhedron of the Eu(III) atom is a distorted dodecahedron. Possible reasons for spectral differences in the Stark structure of photo-and triboluminescence of I are discussed. 相似文献
15.
The crystalline structure of a new compound Rh(III) of (NH4)2[Rh(NO2)3(NH3)(μ-OH)]2 composition has been determined. The crystallographic characteristics are H16N10O14Rh2: a = 6.3963(2) Å, b = 9.3701(4) Å, c = 13.6646(5) Å, β = 102.266(1)°, V = 800.28(5) Å3, Z = 2, d
calc = 2.432 g/cm3. The distance Rh...Rh in the dimer is 3.200 Å.
Original Russian Text Copyright ? 2006 by S. P. Khranenko, I. A. Baidina, and S. A. Gromilov
__________
Translated from Zhurnal Strukturnoi Khimii, Vol. 47, No. 2, pp. 380–384, March–April, 2006. 相似文献
16.
Yu. V. Kokunov Yu. E. Gorbunova L. V. Khmelevskaya 《Russian Journal of Inorganic Chemistry》2006,51(8):1192-1197
The compound [Ag(Bpe)](NO3)·3H2O (Bpe = 4,4′-bipyridylethylene, C12H10N2) is prepared and its crystal structure is determined. The crystals are triclinic: a = 9.073(2) Å, b = 10.074(2) Å, c = 10.391(2) Å, α = 61.18(3)°, β = 72.11(3)°, γ = 68.62(3)°, space group P $\bar 1$ , V = 764.7(3) Å3, ρ(calcd) = 1.764 g/cm3, Z = 2. The structure is composed of polymeric cationic chains, [Ag(Bpe)] ∞ + , NO 3 ? counterions, and water molecules. The Ag+ ions are bound to the two N atoms of two crystallographically nonequivalent Bpe ligands and form a nearly linear coordination (Ag(1)-N(1), 2.129 Å; Ag(1)-N(2), 2.120(4) Å; N(1)Ag(1)N(2), 169.9(2)°). 相似文献
17.
V. I. Belomestnykh L. B. Sveshnikova Yu. N. Mikhailov 《Russian Journal of Inorganic Chemistry》2013,58(6):664-670
The reaction of diaquadinitratouranyl with ammonium nitrate in ethanol gave the single crystals of ((NH4)2[}UO2(NO3)2}2(μ4-C2O4)] · 2H2O (I).The structure of the complex was studied by X-ray diffraction. The crystals are monoclinic, a = 8.6497(10) Å, b = 11.7001(10) Å, c = 20.2135(10) Å, β = 93.924(10)°, space group P21/c, Z = 4, V = 2040.9(3) Å3. The structural units of the crystal are island binuclear groups [{UO2(NO3)2}2(μ4-C2O4)]2?, ammonium cations, and crystal water molecules. The structure has a complex three-dimensional packing provided by electrostatic attraction forces of the counterions and the hydrogen bond system involving water molecules, oxalate, nitrate, and uranyl ions. The IR spectra of I confirm the X-ray diffraction data. 相似文献
18.
A. N. Chekhlov 《Russian Journal of Inorganic Chemistry》2007,52(3):378-382
A crystalline adduct of 2.2.2-cryptand and nitric acid, [H2(Crypt-222)]2+·2(NO 3 ? ·HNO3) (I), is synthesized and studied using X-ray diffraction analysis. The monoclinic structure of compound I (space group C2/c, a = 13.326 Å, b = 15.262 Å, c = 15.020 Å, β = 98.96°, Z = 4) is solved by a direct method and refined by the full-matrix least-squares method in the anisotropic approximation to R = 0.067 for 2647 independent reflections (CAD4 automated diffractometer, λMoK α radiation). In the structure of compound I, the 2.2.2-cryptand dication lies on an axis 2 and has an endo-endo conformation, for which two H atoms at two protonated N atoms are directed inside the cavity. One of the NO 3 ? ·HNO3 dimers is situated in the inversion center, and the other dimer lies on another axis 2 and is disordered over three orientations. All H atoms in the NO 3 ? ·HNO3 dimers are equiprobably disordered over two close sites. Each of the two NO 3 ? ·HNO3 dimers is formed by the very strong disordered N-O-H···O=N hydrogen bond between the nitric acid molecule and nitrate anion. 相似文献
19.
A. N. Chekhlov 《Russian Journal of Inorganic Chemistry》2006,51(2):235-240
A new complex, (2.2.2-cryptand)(nitrato-O,O’)lead(II) nitrate monohydrate [Pb(NO3)(Crypt-222)]+ · NO 3 ? · H2O, is synthesized and characterized by X-ray crystallography. The structure of the complex (space group Pbca, a = 14.196 Å, b = 14.001 Å, c = 26.745 Å, Z = 8) is solved by direct methods and refined by the full-matrix least-squares method in the anisotropic approximation to R = 0.073 for 3474 unique reflections (CAD4 automated diffractometer, λMOK α). The structure contains the host-guest complex cation [Pb(NO3)(Crypt-222)]+. The Pb2+ cation is located in the cavity of the 2.2.2-cryptand ligand and is coordinated by all eight heteroatoms (6O + 2N) of the cryptand ligand and two O atoms of the NO 3 ? ligand. The coordination polyhedron of the Pb2+ cation (ten-coordinate) is a strongly distorted hexagonal bipyramid with a base of four O atoms and two N atoms of the cryptand ligand and with two bifurcated axial vertices at two O atoms of the nitrate ligand and two O atoms of the cryptand ligand. The disordered NO 3 ? anion and the water molecule are linked by hydrogen bonds. 相似文献
20.
Matthias Weil 《无机化学与普通化学杂志》2005,631(8):1346-1348
Light‐yellow single crystals of the mixed‐valent mercury‐rich basic nitrate Hg8O4(OH)(NO3)5 were obtained as a by‐product at 85 °C from a melt consisting of stoichiometric amounts of (HgI2)(NO3)2·2H2O and HgII(OH)(NO3). The title compound, represented by the more detailed formula HgI2(NO3)2·HgII(OH)(NO3)·HgII(NO3)2·4HgIIO, exhibits a new structure type (monoclinic, C2/c, Z = 4, a = 6.7708(7), b = 11.6692(11), c = 24.492(2) Å, β = 96.851(2)°, 2920 structure factors, 178 parameters, R1[F2 > 2σ(F2)] = 0.0316) and is made up of almost linear [O‐HgII‐O] and [O‐HgI‐HgI‐O] building blocks with typical HgII‐O distances around 2.06Å and a HgI‐O distance of 2.13Å. The Hg22+ dumbbell exhibits a characteristic Hg‐Hg distance of 2.5079(7) Å. The different types of mercury‐oxygen units form a complex three‐dimensional network exhibiting large cavities which are occupied by the nitrate groups. The NO3? anions show only weak interactions between the nitrate oxygen atoms and the mercury atoms which are at distances > 2.6Å from one another. One of the three crystallographically independent nitrate groups is disordered. 相似文献