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1.
Single crystals of diammonium tetranitratouranylate (NH4)2[UO2(NO3)4] (I) and a new diammonium tetranitratouranylate complex with 18-crown-6 [(NH4)(18C6)]2[UO2(NO3)4] (II) have been synthesized by the reaction of diaquadinitratouranyl tetrahydrate with ammonium nitrate in a nitric acid solution and the reaction of the same reagents with 18C6 in an ethanol solution, respectively. The X-ray diffraction analysis of compounds I and II has been performed. Crystals of compounds I and II are monoclinic, Z = 2, space group P21/n, a = 6.4075(5) ?, b = 7.7851(7) ?, c = 12.4461(12) ?, β = 101.239(1)°, V = 608. 94(9) ?3 for compound I and a = 10.542(9) ?, b = 8.590(8) ?, c = 22.5019(19) ?, β = 101.632(1)°, V = 2058.3(3) ?3 for compound II. The [UO2(NO3)4]2− complex anion in compounds I and II contains two monodentate and two bidentate cyclic nitrato groups, and the coordination number of uranyl is 6. The 18C6 molecule in the structure of compound II has the classic crown conformation and combined with the ammonium ion by three hydrogen bonds. Compounds I and II formed by electrostatic attraction forces between counterions are stabilized by (NH4+)NH...O(NO3) interionic hydrogen bonds.  相似文献   

2.
The interaction of the Co(iso-Bu2PS2)2 chelate with 4-NH2Py afforded a paramagnetic complex [Co(4-NH2Py)(iso-Bu2PS2)2] (μeff = 4.53 BM). Single crystals of [Ni(4-NH2Py)2(iso-Bu2PS2)2] (I) and [Co(4-NH2Py)(iso-Bu2PS2)2] (II) were grown and used for X-ray diffraction investigation (X8 APEX diffractometer, MoK α radiation). Crystals I are monoclinic with unit cell parameters a = 12.5336(5) Å, b = 9.4356(4) Å, c = 16.4095(6) Å; β = 111.351(1)°; V = 1807.4(1) Å3; Z = 2, ρ = 1.223 g/cm3, space group P21/n. Crystals II are triclinic with unit cell parameters a = 8.7572(4) Å, b = 9.6934(6) Å, c = 18.665(1) Å; α = 79.374(2)°, β = 87.049(2)°, γ = 75.640(2)°; V = 1508.6(1) Å3; Z = 2, ρ = 1.259 g/cm3; space group . The structures of I and II are formed by isolated mononuclear molecules. The coordination unit is NiN2S4 (octahedron) in I and CoNS4 (tetragonal pyramid) in II. The 4-NH2Py molecule is coordinated through the N atom of the heterocycle. Electronic spectroscopy data for II agree with the symmetry of the NS4 polyhedron found by X-ray diffraction (XRD) analysis. The noncoordinated amine groups link the complex molecules via N-H...S hydrogen bonds. __________ Translated from Zhurnal Strukturnoi Khimii, Vol. 46, No. 6, pp.1072–1080, November–December, 2005. Original Russian Text Copyright ? 2005 by T. E. Kokina, L. A. Glinskaya, E. A. Sankova, R. F. Klevtsova, and S. V. Larionov  相似文献   

3.
Double complex salts (DCSs) [Co(NH3)6][Fe(CN)6] (I) and [Co(NH3)6]2[Cu(C2O4)2]3 (II) and complex [Co(NH3)6]2(C2O4)3·4H2O (III) are synthesized and investigated by single crystal XRD, crystal optics, and elemental analysis. The crystalline phases of I, II, and III (R-3, P21/c, and Pnnm space groups respectively) have the following crystallographic characteristics: a = 10.9804(2) ?, b = 10.9804(2) ?, c = 10.8224(3) ?, V = 1130.03(4) ?3, Z = 3, d x = 1.65 g/cm3 (I); a = 9.6370(2) ?, b = 10.2452(2) ?, c = 13.2108(3) ?, V = 1932.90(9) ?3, Z = 2, d x= 1.97 g/cm3 (II), and a = 11.7658(3) ?, b = 11.7254(3) ?, c = 14.1913(4) ?, V = 1304.34(5) ?3, Z = 2, d x = 1.68 g/cm3 (III). This paper investigates the products of DCS thermolysis in a hydrogen atmosphere: the intermetallic compound CoFe with the bcc parameter a = 2.852 ? for I and a heterogeneous mixture of Co and Cu in the decomposition of II. The coordinated CN and C2O42− groups then turn into NH3, hydrocarbons, and CO2. The dominant hydrocarbon is methane.  相似文献   

4.
Uranyl complexes with acetylenedicarboxylic acid, K(H5O2)[UO2L2H2O] · 2H2O (I) and Cs2[UO2L2H2O] · 2H2O (II), L2− = C4O 4 2− were prepared for the first time. The composition and structure of the complexes were determined by X-ray diffraction. The crystal data are as follows: a = 16.254(12) ?, b = 13.508(8) ?, c = 7.683(6) ?, β = 90.91(7)°, space group C2/c, V = 1687(2) ?3 (I); a = 7.0745(10), b = 18.4246(10), c = 13.1383(10) ?, space group Abm2, V = 1712.5(3) ?3 (II). The structures of I and II are based on [UO2L2H2O] n 2− anionic chains stretched along the [101] direction (I) or [010] direction (II). In I and II, the uranium coordination polyhedron is a pentagonal bipyramid in which the equatorial environment of the uranyl ions is formed by the oxygen atoms of the four L2− anions and the water molecule. The L2− anions in I and II are bidentate bridging ligands connecting two uranium atoms that are next to each other in the anionic chain; their coordination capacity is equal to 2. In I, the K+ and H5O 2 + cations are outer-sphere species. The latter form hydrogen bonds combining the anionic chains shifted by translation b with respect to each other. The [UO2L2H2O] n 2− chains in I are surrounded by the potassium and oxonium cations; in II, these are combined by hydrogen bonds into anionic layers between which Cs+ cations are arranged. The IR spectrum of compound II was measured and interpreted. Original Russian Text ? I.A. Charushnikova, A.M. Fedoseev, N.A. Budantseva, I.N. Polyakova, Ph. Moisy, 2007, published in Koordinatsionnaya Khimiya, 2007, Vol. 33, No. 1, pp. 63–69.  相似文献   

5.
Heterometallic chloride complexes [Mo5NbI8Cl6] n (n = 2, 3) are synthesized. The crystal structures of their salts are determined: for (Ph4P)2[Mo5NbI8Cl6] (I), triclinic crystal system, spacegroup P [`1]\bar 1, a = 10.9886(6), b = 11.4604(5), c = 13.4343(7) ?, α = 66.124(2), β = 86.892(2), γ = 86.490(2)°, Z = 1, V = 1543.35(13) ?3; and for (4-MePyH)5[Mo5NbI8Cl6]Cl2 (II), monoclinic crystal system, space group C2/m, a = 16.4937(4), b = 14.7335(3), c = 11.6534(3) ?, β = 99.8750(10)°, Z = 2, V = 2789.94(11) ? The geometric parameters of compounds I and II and the conditions for the formation of the complexes with the charges −2 and −3 are discussed.  相似文献   

6.
Triphenylbismuth diaroxides Ph3Bi(OAr)2 (Ar = C6H3(Br2-2,4) (I), C6H2(Br2-2,6)(NO2-4) (II), and C6H2[(NO2)3-2,4,6] (III) are synthesized in yields up to 74% by the reaction of triphenylbismuth with phenols in the presence of hydrogen peroxide (taken at a molar ratio 1: 2: 1, respectively) in ether. According to X-ray diffraction data, the bismuth atoms in compounds I-III have distorted trigonal-bipyramidal coordination with the aroxyl substituents in the axial positions; the Bi-C, Bi-O bond lengths and the OBiO, CBiC angles vary in the intervals 2.162–2.204, 2.150–2.299 ? and 172.4°–176.1°, 109.6°–139.9°, respectively. Compound II exhibits intramolecular contacts between the central atom and ortho-Br atoms (3.924, 4.101 ?), and compound III has similar contacts of the Bi atom with the O atoms of the ortho-nitro groups (3.114, 3.313 ?). Original Russian Text ? V.V. Sharutin, I.V. Egorova, O.K. Sharutina, A.P. Pakusina, M.A. Pushilin, 2007, published in Koordinatsionnaya Khimiya, 2007, Vol. 33, No. 1, pp. 14–21.  相似文献   

7.
Coordination polymers [Ag(Me4Pyz)] PF6(I) and [Ag2(Me4Pyz)3](BF4)2·H2O (II) have been synthesized, and their structures have been determined. The crystals of I are monoclinic, space group C2/c, a = 9.440(2) ?, b = 10.587(2) ?, c = 13.165(3) ?, β= 107.19(3)°, V = 1257.0(5) ?3, d = 2.056 g/cm3, Z = 4. The crystals of II are monoclinic, space group P21/n, a = 13.062(3) ?, b = 12.259(2) ?, c = 18.996(4) ?, β = 97.73(3)°, V = 3014.1(11)?3, ρ = 1.798 g/cm3, Z = 4. The structure of I is built of linear polymeric cations [Ag(C8H12N2)] + and octahedral anions [PF6]. Upon the interaction of tetramethylpyrazine molecule with Ag+ ions, intersecting polymeric chains [Ag(C8H12)] + (1D polymer) are formed extending in mutually perpendicular diagonal directions. The structure of II consists of layers (2D polymers) formed by fused sixmembered rings. These rings consist of Ag+ ions linked by bridging ligands Me4Pyz. Original Russian Text ? Yu.V. Kokunov, Yu.E. Gorbunova, 2007, published in Zhurnal Neorganicheskoi Khimii, 2007, Vol. 52, No. 5, pp. 743–750.  相似文献   

8.
The heteroligand complex Nd(Phen){(iso-C4H9)2PS2}2(NO3) (I) was synthesized and its IR spectrum was analyzed. The anions (iso-C4H9)2PS2/− and N3/− act as bidentate cyclic ligands. The single crystals of [Nd(Phen){iso-C4H9)2PS2}3] (II) were obtained on evaporation of a solution of complex I in a mixture CH2Cl2-hexane and were studied by X-ray diffraction. Crystals II are triclinic: a = 10.5509(5); b = 14.7432(8), c = 16.8503(10) ?; α = 102.882(2)°, β = 97.211(2)°, γ= 108.087(2)°, V = 2374(2) ?3, Z = 2, ρ(calcd.) = 1.332 g/cm3, space group . The coordination polyhedron of the Nd atom in a separate mononuclear molecule II is a distorted dodecahedron N2S6. The molecules are bound by weak van der Waals and π-π interactions. The photoluminescence spectra of complexes I, II were measured and interpreted. Original Russian Text ? S.V. Larionov, V.L. Varand, R.F. Klevtsova, T.G. Leonova, L.A. Glinskaya, E.M. Uskov, 2008, published in Koordinatsionnaya Khimiya, 2008, Vol. 34, No. 12, pp. 944–950.  相似文献   

9.
New complex chlorides [ZnCl2(ODA)] (I) (ODA=oxydianiline, C12H12N2O) and [ZnCl2(H2O)2](Me4Pyz)2 (II) (Me4Pyz = 2,3,5,6-tetramethylpyrazine) were synthesized and crystallographically characterized. Crystals of I are monoclinic, space group C2/c, a = 22.682(2) ?, b = 12.646(1) ?, c = 9.951(1) ?, β = 93.23(2)°, V = 2849.7(5) ?3, ρcalc = 1.569 g/cm3, Z = 8. Structure I contains cyclic fragments consisting of two tetrahedral complexes (ZnCl2N2) and two coordinated bridging oxydianiline ligands. Crystals of II are monoclinic, space group P2(1)/c, a = 8.972(2) ?, b = 13.862(3) ?, c = 17.528(4) ?, β = 101.72(3)°, V = 2134.5(7) ?3, ρcalc = 1.384 g/cm3, Z = 4. In structure II, supramolecular pseudo-metallocycles are formed due to formation of hydrogen bonds O(w)-H…N between coordinated water molecules and noncoordinated nitrogen atoms of tetramethylpyrazine molecules.  相似文献   

10.
A new compound [MNII(Phen)3]2+(B6H7)2 is synthesized; its crystal structure is studied by XRD at 100 K. Crystallographic data: C36H38B12N6Mn, M = 739.39, triclinic symmetry, space group P , unit cell parameters: a = 10.3131(3) ?, b = 13.4839(4) ?, c = 15.1132(4) ?; α = 97.696(1)°, β = 108.324(1)°, γ = 102.211(1)°; V = 1903.9(1) ?3, Z = 2, d calc = 1.290 g/cm3. The structure is solved by direct and Fourier methods and refined by full-matrix LSM in the anisotropic (isotropic for hydrogen atoms) approximation to the final factor R 1 = 0.036 for 10169 I hkl ≥ 2σ I (Bruker-Nonius X8 APEX CCD diffractometer, λMoK α). The structure contains two crystallographically different anions. Original Russian Text Copyright ? 2009 by T. M. Polyanskaya, M. K. Drozdova, V. V. Volkov, and K. G. Myakishev __________ Translated from Zhurnal Strukturnoi Khimii, Vol. 50, No. 2, pp. 381–385, March–April, 2009.  相似文献   

11.
A new binuclear cadmium(II) complex with neutral ligands, 1,2-diaminobenzene (DMB) and dimethylformamide (DMF), [Cd2(Ph(NH2)2)5(DMFA)4](B10H10)2, was synthesized and studied by IR spectroscopy and X-ray diffraction. The crystals are monoclinic, a = 26.198(3) ?, b = 12.742(3) ?, c = 21.658(3) ?, β = 119.985(10)°, Z = 8, space group C2/c. The distorted octahedral environment of Cd is formed by four nitrogen atoms of three DAB molecules and two oxygen atoms of DMF molecules. Three independent DAB molecules perform different functions: one chelates the Cd atom, another is linked to cadmium as a monodentate ligand, and the third one bridges two Cd atoms, thus forming the dimer. The amino groups of the DAB molecules are involved in the N-H⋯O and N-H⋯N hydrogen bonds and in N-H⋯B and N-H⋯H-B specific interactions with the cluster boron anion. Original Russian Text ? E.A. Malinina, V.V. Drozdova, L.V. Goeva, I.N. Polyakova, N.T. Kuznetsov, 2007, published in Zhurnal Neorganicheskoi Khimii, 2007, Vol. 52, No. 6, pp. 922–926.  相似文献   

12.
Two copper(I) complexes [Cu(Cin2bda)2]ClO4 (I) and [Cu(Ncin2bda)2]ClO4 (II) have been prepared by the reaction of the ligands N2,N2′-bis(3-phenylallylidene)biphenyl-2,2′-diamine (L1) and N2,N2′-bis[3-(2-nitrophenyl)allylidene]biphenyl-2,2′-diamine (L2) and copper(I) salt. These compounds were characterized by CHN analyses, 1H NMR, IR, and UV-Vis spectroscopy. The C=N stretching frequency in the copper(I) complexes shows a shift to a lower frequency relative to the free ligand due to the coordination of the nitrogen atoms. The crystal and molecular structure of II was determined by X-ray single-crystal crystallography. The coordination polyhedron about the copper(I) center in the complex is best described as a distorted tetrahedron. A quasireversible redox behavior was observed for complexes I and II. The article is published in the original.  相似文献   

13.
The coordination compound [Cu33-OH)(μ-L)3(NO3)2(H2O)] · 2H2O (I), where L is the α-(3,3-dimethyl-3,4-dihydro-1-isoquinolyl)hydroxyiminoacetonitrile anion, has been synthesized. The crystal and molecular structure of I was determined by X-ray diffraction (Enraf-Nonius CAD4, MoK α radiation, graphite monochromator, ω-scan mode, 2θmax = 49.96°, 7673 unique reflections, a = 12.745(3) ?, b = 13.726(3) ?, c = 28.835(6) ?, β = 93.44(3)°, V = 5035.2(17) ?3, Z = 4, space group P21/c). In the trimer complex I, the copper atoms are combined by a bridging hydroxy group. The copper atoms are additionally linked pairswise by three tridentate chelating bridging organic anions coordinated to the Cu(II) atoms by the N and O atoms of the deprotonated oxime group and by the N atom of the dihydroisoquinoline moiety. Original Russian Text ? V.I. Sokol, V.V. Davydov, N. Yu. Merkur’eva, E.I. Polyakova, Yu.V. Shklyaev, V.S. Sergienko, 2007, published in Zhurnal Neorganicheskoi Khimii, 2007, Vol. 52, No. 10, pp. 1643–1652.  相似文献   

14.
The double complex salts [Ru(NH3)5Cl][PtCl6] (I) and [Ru(NH3)5Cl]2[PtCl6]Cl2 (II) were synthesized and studied by X-ray diffraction. They were found to be isostructural to the previously synthesized [Rh(NH3)5Cl][OsCl6] and [Ir(NH3)5Cl]2[PtCl6]Cl2. The thermolysis of the complexes in the atmosphere of hydrogen and helium was studied by the powder X-ray diffraction analysis. The product of the salt I thermolysis is a single-phase solid solution Ru0.5Pt0.5 (a = 3.857(3) ?), the thermolysis of salt II results in a double-phase metallic powder. Original Russian Text ? S.A. Martynova, K.V. Yusenko, I.V. Korol’kov, S.A. Gromilov, 2007, published in Koordinatsionnaya Khimiya, 2007, Vol. 33, No. 7, pp. 541–545.  相似文献   

15.
An XRD analysis is used to study the single crystal of [Pd(NH3)4][Rh(NH3)(NO2)5] double complex salt at T = 150(2) K. Crystallographic characteristics are as follows: a = 7.6458(5) ?, b = 9.8813(6) ?, c = 9.5788(7) ?, β = 109.469(2)°, V = 682.30(8) ?3, P21/m space group, Z = 2, d x = 2.553 g/cm3. The geometry of the complex [Rh(NH3)(NO2)5]2− anion is described for the first time: Rh-N(NO2) distances are 2.020(4)–2.060(3) ?, Rh-N(NH3) 2.074(4) ?, N(NO2)-Rh-N(NH3) trans-angle is 178.8(2)°.  相似文献   

16.
The interaction of binuclear cadmium dialkyldithiocarbamates [Cd2(S2CNR2)4] with solutions of AuCl3 in 2M HCl gives polynuclear gold(III) complexes ([Au(S2CNR2)2][AuCl4]) n , where R = C4H9 (I) and R2 = (CH2)5 (II). The structures of the synthesized compounds solved by X-ray diffraction analysis are char-acterized by a complicated organization at the supramolecular level. The structures are based on polymer chains (I) and layers (II) involving isomeric cations [Au(S2CNR2)2]+ and anions [AuCl4]. The thermal behavior of the synthesized complexes is studied by simultaneous thermal analysis including thermogravimetry and differential scanning calorimetry. The final product of the thermal transformations of the studied complexes is shown to be reduced metallic gold.  相似文献   

17.
Single crystals of the solid solutions CdGeAs2:Mn(x) and Cd0.964Zn0.036GeAs2:Mn(x) have been grown by the vertical Bridgman method. An X-ray diffraction study has demonstrated that Cd0.964Zn0.036GeAs2 (I), Cd0.964Zn0.036GeAs2:Mn (1.5 wt%) (II), and Cd0.964Zn0.036GeAs2:Mn (2.18 wt %) (III) retain the CdGeAs2 structure (tetragonal system, space group I 2d). The unit cell parameters of the solid solutions are as follows: a = b = 5.934(1) ?, c = 11.219(2) ? for I; a = b = 5.919(1) ?, c = 11.204(2) ? for II; and a = b = 5.918(1) ?, c = 11.208(2) ? for III. Many of Mn atoms in II and III occupy interstitial sites in the crystal lattice. Selected electrical and magnetic properties of single crystals of CdGeAs2:Mn(x) are discussed. Original Russian Text ? S.G. Mikhailov, K.K. Palkina, A.V. Molchanov, S.F. Marenkin, T.V. Filippova, L.I. Ochertyanova, I.S. Zakharov, A.V. Kochura, R. Laiho, E. Lahderanta, A. Lashkul, M.A. Shakhov, 2007, published in Zhurnal Neorganicheskoi Khimii, 2007, Vol. 52, No. 11, pp. 1879–1885.  相似文献   

18.
The crystals of [C9H7NC3H5]Cu(SCN)2 (I) and [C9H7NC3H5]Cu2(SCN)3 (II) were obtained in the reaction of N-allylquinolinium bromide with CuSCN and NH4SCN in a methanol solution. The crystals of I are triclinic: space group P , Z = 2, a = 8.619(2), b = 8.755(2), c = 10.463(3) ?, α = 77.18(3), β = 69.95(3), γ = 79.38(3)°, V = 718.1(3) ?3. The crystals of II are opthorhombic: space group P212121, Z = 4, a = 5.744(2), b = 16.799(4), c = 17.980(5), V = 1735.9(9) ?3. The structure of compound I is built of infinite linear {Cu(SCN)2} anions and the N-allylquinolinium cations bonded additionally by relatively weak hydrogen contacts C-H...S. The [C9H7NC3H5]+ cations are located between the corrugated layers of the {Cu2(SCN)3} anions in compound II. As in the case of the previously studied copper(I) halide complexes, the C=C bond of the allyl group in the N-allylquinolinium cation of complexes I, II does not interact with Cu(I). Original Russian Text ? A.V. Pavlyuk, V. Kinzhybalo, T. Lis, M.G. Mys’kiv, 2008, published in Koordinatsionnaya Khimiya, 2008, Vol. 34, No. 10, pp. 764–769.  相似文献   

19.
A solvothermal reaction of 2-pyrazinic acid with Zn(SO4)2 · 7H2O yielded the title complex of the formula {[Zn2(Pyz)2(H2O)4] · SO4} n (I). X-ray diffraction study shows that the complex I crystallizes in mono-clinic system, space group P21/c, with lattice parameters a = 11.2687(6), b = 7.3511(4), c = 11.8506(7) ?, β = 95.070(2)°, V = 977.83(9) ?3, Z = 4, and ρcalcd = 2.184 mg m−3.  相似文献   

20.
Single crystals of (H3O)[UO2(CH3COO)3] (I) and (NH(C2H5)3)[UO2(CH3COO)3] (II) are synthesized, and their structures are studied by X-ray crystallography. Compound I crystallizes in the tetragonal crystal system with the unit cell parameters a = 13.70640(10) ?, c = 27.5258(5) ?, V = 5171.14(11) ?3, space group I41/a, Z = 16, R = 0.0238. The crystals of compound II are orthorhombic with the parameters a = 13.3685(3) ?, b = 10.6990(3) ?, c = 12.2616(3) ?, V = 1753.77(8) ?3, space group Pna21, Z = 4, R = 0.0228. The uranium-containing structural units of crystals I and II are [UO2(CH3COO)3] island mononuclear groups belonging to the A B301(A = UO22+, B01 = CH3COO) crystal-chemical group of uranyl complexes. [UO2(CH3COO)3] complexes are linked into a three-dimensional framework by electrostatic interactions with the outer-sphere cations and by hydrogen bonds involving the hydrogen atoms of hydroxonium (I) or triethylammonium (II) with the oxygen atoms of the acetato groups.  相似文献   

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