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1.
The title complexes, K[SmIII(Edta)(H2O)3] · 2H2O(I)(H4Edta = ethylenediamine-N,N,N′,N′-tetraacetic acid) and K2[SmIII(Pdta)(H2O)2]2 · 4.5H2O (II) (H4Pdta = propylenediamine-N,N,N′,N′-tetraacetic acid), were prepared and their compositions and structures were determined by elemental analyses and single-crystal X-ray diffraction techniques, respectively. Complex I has a mononuclear structure, and the Sm3+ ion is nine-coordinated by an Edta ligand and three water molecules, yielding a pseudo-monocapped square antiprismatic conformation, and the complex crystallizes in the orthorhombic crystal system with space group Fdd2. The crystal data are as follows: a = 19.84(5), b = 35.58(9), c = 12.15(3) ?, V = 8580(38) ?3, Z = 16, ρ c = 1.925 g/cm3, μ = 3.010 mm−1, F(000) = 4976, R = 0.0252, and wR = 0.0560 for 3510 observed reflections with I ≥ 2σ(I). Complex II has a binuclear structure and the Sm3+ ion is ten-coordinated by a Pdta ligand, two oxygen atoms from a carboxylic group of adjacent Pdta ligand and two water molecules, yielding a distorted bicapped square antiprismatic prism. The complex crystallizes in the triclinic crystal system with space group P $ \bar 1 $ \bar 1 . The crystal data are as follows: a = 8.9523(15), b = 10.7106(15), c = 11.6900(19) ?, α = 80.613(5)°, β = 80.397(5)°, γ = 76.530(4)°, V = 1065.7(3) ?3, Z = 1, ρc = 1.970 g/cm3, μ = 2.532 mm−1, F(000) = 1620, R = 0.0332 and wR = 0.0924 for 5390 observed reflections with I ≥ 2σ(I).  相似文献   

2.
In this work, the title complexes, NH4[ErIII(Cydta)(H2O)2] · 4.5H2O (I) (H4Cydta = trans-1,2-cyclo-hexanediamine-N,N,N′,N′-tetraacetic acid) and (NH4)2[Er2III(Pdta)2(H2O)2] · 2H2O (II) (H4Pdta= propylene-diamine-N,N,N′,N′-tetraacetic acid), were prepared, respectively, and their composition and structures were determined by elemental analyses and single-crystal X-ray diffraction techniques. Complex I selects a mononu-clear structure with pseudosquare antiprismatic geometry crystallized in the triclinic crystal system with space group $ P\bar 1 $ P\bar 1 and the central Er3+ ion is eight-coordinated by the hexadentate Cydta ligand and two water molecules. The crystal data are as follows: a = 8.568(3), b = 10.024(3), c = 14.377(4) ?, α = 88.404(4)°, β = 75.411(4)°, γ = 88.332(4)°, V = 1194.2(6) ?3, Z = 1, ρ c = 1.793 g/cm3, μ = 3.586 mm−1, F(000) = 648, R = 0.0257, and wR = 0.0667 for 4169 observed reflections with I ≥ 2σ(I). Complex II is eight-coordinated as well, which selects a binuclear structure with two pseudosquare antiprismatic geometry and crystallizes in the monoclinic crystal system with space group P21/n. The central Er3+ ion is coordinated by two nitrogens and four oxygens from one hexadentate Pdta ligand. Besides, two oxygens come from one carboxylic group of the neighboring Pdta ligand and one water molecule, respectively. The crystal data are as follows: a = 12.7576(8), b = 9.3151(6), c = 14.3278(9) ?, β = 96.1380(10)°, V = 1692.93(19) ?3, Z = 4, ρ c = 2.054 g/cm3, μ = 5.015 mm−1, F(000) = 1028, R= 0.0228, and wR = 0.0534 for 2984 observed reflections with I ≥ 2σ(I).  相似文献   

3.
Methods for the synthesis of trans-diammino complexes [RuNO(NH3)2(NO2)2(OH)] (I) and [RuNO(NH3)2(H2O)(NO3)2](NO3)·H2O (II) are suggested. The compounds were studied by IR spectroscopy and X-ray phase and X-ray structural analyses. Crystal data: space group P-1; a = 6.2328(2) ?, b = 11.0488(3) ?, c = 11.0981(4) ?, α = 71.942(1)°, β = 83.291(1)°, γ = 86.877(1)° (I); space group P21; a = 6.6290(2) ?, b = 13.4389(5) ?, c = 7.0180(2) ?, β 114.281(1)° (II). Complex II readily lost some part of crystal water on storage in open air. Original Russian Text Copyright ? 2009 by M. A. Il’in, E. V. Kabin, V. A. Emel’yanov, I. A. Baidina, and V. A. Vorob’yov __________ Translated from Zhurnal Strukturnoi Khimii, Vol. 50, No. 2, pp. 341–348, March–April, 2009.  相似文献   

4.
A single crystal of [Pd(NH3)4]3[Ir(NO2)6]2·H2O double complex salt is studied by X-ray diffraction. Crystallographic characteristics are as follows: a = 21.0335(5) ?, b = 8.0592(2) ?, c = 21.3452(5) ?, β = 91.254(1)°, V = 3617.43(15) ?3, P21/c space group, Z = 4, d x = 2.714 g/cm3. Single-layer pseudohexagonal packing of complex anions is determined along the [−1 0 1] direction in the structure. Complex cations and crystallization water molecules are located between the mentioned layers.  相似文献   

5.
The title complexes, K[Dy(Edta)(H2O)3] · 3.5 H2O (I) (H4Edta = ethylenediamine-N,N,N′,N′-tetraacetic acid), (NH4)3[Dy(Ttha)] · 5H2O (II) (H6Ttha = triethylenetetramine-N, N,N′,N″,N‴,N‴-hexaacetic acid), and NH4[Dy(Cydta)(H2O)2] · 4.5H2O (III) (H4Cydta = trans-1,2-cyclohexanediamine-N,N,N′,N′-tetraacetic acid), were prepared, and their compositions and structures were determined by elemental analyses and single-crystal X-ray diffraction techniques, respectively. In complex I, the Dy3+ ion is nine-coordinated by an Edta ligand and three water molecules, yielding a pseudo-monocapped square antiprismatic conformation, and the complex crystallizes in the orthorhombic crystal system with space group Fdd2. The crystal data are as follows: a = 19.751(7), b = 35.573(12), c = 12.227(4) ?, V = 8591(5) ?3, Z = 16, space group Fdd2 ρc = 1.877 g/cm3, μ = 3.742 mm−1, F(000) = 4800, R = 0.0259, and wR = 0.0616 for 3218 observed reflections with I ≥ 2σ(I). For complex II, the Dy3+ ion is nine-coordinated by a Ttha ligand, yielding a pseudo-monocapped square antiprismatic conformation, and the complex crystallizes in the monoclinic crystal system with space group P21/c. In addition, there is a free non-coordinate carboxyl group (-CH2COO) in the [Dy(Ttha)]3− complex anion. The crystal data are as follows: a = 10.353(3), b = 12.746(4), c = 23.141(7) ?, β = 91.005(5)°, V = 3053.2(15) ?3, Z = 4, space group P21/c ρc = 1.730 g/cm3, μ = 2.532 mm−1, F(000) = 1620, R = 0.0332 and wR = 0.0924 for 5390 observed reflections with I ≥ 2σ(I). For complex III, the Dy3+ ion is eight-coordinated by a ligand Cydta and two water molecules, yielding a distorted square antiprismatic conformation, and the complex crystallizes in the triclinic system with space group P . The crystal data are as follows: a = 8.604(3), b = 10.012(4), c = 14.369(6) ?, α = 88.330(6)°, β = 75.363(6)°, γ = 88.285(6)°, space group P V = 1196.9(8) ?3, Z = 2, ρc = 1.776 g/cm3, μ = 3.194 mm−1, F(000) = 644, R = 0.0445 and wR = 0.1041 for 3931 observed reflections with I ≥ 2σ(I). The article is published in the original.  相似文献   

6.
A new Pd nitrate complex KCs[Pd(NO3)4]·0.5H2O is synthetized. Its crystal structure contains isolated complex anions [Pd(NO3)4]2−, cations K+, Cs+, and crystallization water. Square-planar coordination around Pd is achieved by oxygen atoms of monodentate nitrate ligands. The coordinated nitrate ligands are all oriented in the same way, in a “basket”-like arrangement. The coordination around Pd is completed to 4+1 by forming Pd...Pd contacts of 3.564 ?. Original Russian Text Copyright ? 2009 by S. P. Khranenko, I. A. Baidina, N. V. Kuratieva, and S. A. Gromilov __________ Translated from Zhurnal Strukturnoi Khimii, Vol. 50, No. 1, pp. 173–176, January–February, 2009.  相似文献   

7.
The crystal structure of Na2[ReCl6]·6H2O is determined. The crystallographic characteristics are as follows: a = 6.6955(2) ?, b = 7.0926(2) ?, c = 8.3667(3) ?; α = 102.567(1)°, β = 98.853(2)°, γ = 107.236(1)°; V = 360.08(2) ?3, P-1 space group, Z = 1, d x = 2.550 g/cm3. The thermal properties of Na2[ReCl6]·6H2O are studied in the hydrogen atmosphere. During the thermolysis of Na2[ReCl6]0.50[PtCl6]0.50·6H2O double complex salt in the hydrogen atmosphere, Re x Pt1−x nanocrystalline solid solutions were obtained.  相似文献   

8.
The reaction of indium thiocyanate with bipyridine (4,4-Bipy) and urotropine (Ur) gave [H2(4,4′-Bipy)][In(H2O)2(NCS)4]2 (I) and [HUr]2[In(H2O)(NCS)5] · 2H2O (II), which were identified using elemental analysis, IR spectra, and thermogravimetric analysis. The thermal decomposition of compound I and II ends at 650 and 640°C, respectively, and gives In2O3. X-Ray diffraction analysis of compound I showed that complex anions in the crystal form chains through O-H…S hydrogen bonds. The anion chains form a close packing of columns with bipyridine cations located in the voids. Original Russian Text ? S.P. Petrosyants, A.B. Ilyukhin, V.A. Ketsko, 2008, published in Zhurnal Neorganicheskoi Khimii, 2008, Vol. 53, No. 6, pp. 951–955.  相似文献   

9.
Comparing the geometry of [UO2(NO3)2(H2O)2] · 2H2O · 18C6 (18C6 = C12H24O6) and IR spectroscopic data, we propose correlations between the conformation of an ethylene oxide unit of 18-crown-6 and the conformation-sensitive frequency in the IR spectrum. Spectral conformational analysis verifies the composition of the 18-crown-6 conformer in the [UO2(NO3)2(H2O)2] · 18C6 complex whose structure is known. The distribution character of hydrogen bonds that retain crown ether molecules in aquanitratouranyl complexes is shown to influence the conformational uniformity of ethylene oxide units of the macrocycle.  相似文献   

10.
The title compound, [Zn(pytpy)2][NO3]2·2H2O (pytpy = 4′-(4-pyridyl)-2,2′: 6′,2″-terpyridine), has been synthesized by the reaction of Zn(NO3)2·6H2O with pytpy, and its crystal structure was determined by single-crystal X-ray diffraction. The crystal belongs to tetragonal space group P43 with a = 0.90873(8) nm, b = 0.90873(8) nm, c = 4.4741(6) nm, V = 3.6946(7) nm3, Z = 4, D c = 1.521 g/cm−3, μ = 0.736 mm−1, F(000) = 1744, R = 0.0871, wR = 0.1302 for 5553 observed reflections with I > 2σ(I). X-ray analysis has revealed that the ZnII ion is surrounded by six N atoms from two pytpy ligands leading to a distorted octahedral geometry. In the crystal structure there are numerous strong intermolecular and intramolecular H-bonds and π-π interactions.  相似文献   

11.
Complexes Zn(H2O)4(L) (I) and Zn(H2O)(L) (II) (H2L = p-HOOCC6F4COOH) are synthesized. Single crystals of compound [Zn(H2O)4(L) · 4H2O] n (III) are grown. According to the X-ray diffraction data, the crystal structure of compound III is built of zigzag chains of coordination polymer Zn(H2O)4(L) and molecules of water of crystallization. The chain contains ions Zn2+, whose octahedral coordination sphere includes the O atoms of four water molecules and two O atoms of the deprotonated carboxyl groups. The chains in structure III are joined by a system of hydrogen bonds of coordinated water molecules and molecules of water of crystallization. The photoluminescence spectrum of H2L exhibits the band with λmax = 368 nm. The spectra of compounds III, I, and II contain bands at 322, 340, and 353 nm, respectively.  相似文献   

12.
The products of the extraction treatment of Rh(III) and Pd(II) nitrate-nitrite solutions are studied. The [Rh(Thio)6](NO3)3·3H2O and [Pd(Thio)4](NO3)2 complex salts are extracted and an X-ray diffraction analysis of single crystals is performed (BRUKER X8 APEX automated diffractometer, MoK a radiation, graphite monochromator, two-dimensional CCD-detector). [Rh(Thio)6](NO3)3·3H2O crystallographic characteristics are as follows: a = 15.1857(3) ?, b = 10.7292(2) ?, c = 18.8524(4) ?, β = 105.165(1)°, P2 1 /c space group, Z =4; [Pd(Thio)4](NO3)2: a = 5.8013(4) ?, b = 7.0981(5) ?, c = 11.4991(8) ?, α = 99.963(2)°, β = 101.410(2)°, γ = 102.229(2)°, P —1 space group, Z = 1.  相似文献   

13.
The complex [mer-In(H2O)3Cl3] · 18C6 (I) was isolated from the InCl3-H2O-Solv-18C6 solutions (Solv = MeOH, EtOH, THF). The second crystallization from mother solutions resulted in [fac-In(H2O)3Cl3] · 18C6 · 2H2O (II). The crystal and molecular structures of isomers I, II were identified by the powder X-ray diffraction, IR, and X-ray diffraction methods. Although complexes I, II have different compositions, they have the chain structure. The thermal decomposition of complexes I, II was studied. Original Russian Text ? A.B. Ilykhin, Zh.V. Dobrokhotova, S.P. Petrosyants, 2008, published in Koordinatsionnaya Khimiya, 2008, Vol. 34, No. 9, pp. 651–656.  相似文献   

14.
The chain coordination polymers [Na2(μ-H2O)(H2O)CB[5]]Cl2 · 6H2O (I), [Na3(μ-H2O)4(H2O)4(CNPy@CB[6])]Cl3 · 8H2O (II), and [Rb2(μ-H2O)2(CNPy@CB[6])]Cl2 · 8H2O (III) were prepared by heating (110°C) of a mixture of sodium or rubidium chloride, cucurbit[n]uril (CB[n], where n = 5, 6), 4-cyanopyridine, and water. According to X-ray diffraction data, binding of polynuclear cations with CB[n] in IIII occurs through coordination of the oxygen atoms of the cucurbit[n]uril portals to alkali metal atoms. Complexes IIII of the above composition isolated to the solid phase as supramolecular compounds with CB[n] were structurally characterized for the first time.  相似文献   

15.
The vanadium(V) complexes K[VO2(SeO4)(H2O)] and K[VO2(SeO4)(H2O)2] · H2O were synthesized using original procedures; their physicochemical properties were studied, and the crystal structure was determined on the basis of X-ray diffraction and neutron diffraction data. The structure of K[VO2(SeO4)(H2O)2] · H2O is composed of VO6 octahedra connected to form infinite chains by bridging SeO4 tetrahedra. Each VO6 tetrahedron has short terminal V-O bonds forming the bent dioxovanadium group VO2+ The unit cell parameters of K[VO2(SeO4)(H2O)2] · H2O are a = 6.4045(1) ?, b = 9.9721(2) ?, c = 6.6104(1) ?, β = 107.183(1)°, V = 403.34 ?3, Z = 2, monoclinic system, space group P21. The complex K[VO2(SeO4)(H2O)] forms a two-dimensional layered structure composed of highly distorted VO6 octahedra having two short terminal V-O bonds and SeO4 groups coordinated simultaneously by three vanadium atoms. This compound crystallizes in the monoclinic system (space group P21/c): a = 7.3783(1) ?, b = 10.5550(2) ?, c = 10.3460(2) ?, β = 131.625(1)°, V = 602.894(5) ?3, Z= 4. The vibrational spectra of the studied compounds are fully consistent with their structural features.  相似文献   

16.
The structures of the crystals of Ba4[trans(N)-Co(Ida)2]3[cis-(N)-Co(Ida)2]2(ClO4)3 · 19.46H2O · 2CH3OH (I) and Ba[trans-(N)-Co(Ida)2]2 · 7H2O (II) (H2Ida is iminodiacetic acid) were determin by X-ray diffraction. The crystals of I containing two geometric isomers of the complex anions [Co(Ida)2] were obtained by a slow cooling of a hot solution, which contained initially only the cis-isomer. One Ba atom in I interacts with the trans-complex and with two cis-complexes to give a three-dimensional framework in crystal I. The positive charge of the last framework is compensated by one more trans-complex and by the perchlorate ions, one of which acts as a bidentate ligand with respect to the Ba atom. The crystals of II are built of the chains with the alternating Ba atoms and the trans-(N)-[Co(Ida)2] anions. The other anions of the same structure are each “suspended” to the Ba atoms of the chain. Original Russian Text ? M. Zabel, A.I. Poznyak, V.I. Pawlowskii, 2008, published in Koordinatsionnaya Khimiya, 2008, Vol. 34, No. 11, pp. 831–836.  相似文献   

17.
Two metal-organic coordination polymers [Cu(bpy)2(H2O)2](NO3)2·4.5C2H5OH (1) and [Cu2(bpy)(H2O)(L-pha) 2](NO3)2·H2O (2) (L-Hpha = L-phenylalanine, bpy = 4,4′-bipyridyl) are prepared by slow evaporation of an aqueous alcoholic solution of copper nitrate, L-phenylalanine, and 4,4′-bipyridyl. The structure and composition of the obtained compounds are determined by single crystal XRD. The framework of compound 1 is positively charged and forms two types of intersecting channels. Compound 2 is a homochiral metal-organic coordination polymer whose structure contains L-phenylalanine anions.  相似文献   

18.
The NH4[EuIII(Cydta)(H2O)2]·4.5H2O (I) (H4Cydta = trans-1,2-cyclohexanediamine-N,N,N′,N′-tetraacetic acid) and K2[Eu2III(pdta)2(H2O)2]·6H2O (II) (H4pdta = propylenediamine-N,N,N′,N′-tetraacetic acid) complexes are prepared by heat-refluxing and acidity-adjusting methods respectively, and their composition and structures are determined by elemental analyses and single crystal X-ray diffraction techniques. The complex I has a mononuclear structure, crystallizes in the triclinic crystal system with the P[`1]P\bar 1 space group; the central EuIII ion is eight-coordinated by a hexadentate Cydta ligand and two water molecules. The crystal data are as follows: a = 8.653(4) ?, b = 10.041(4) ?, c = 14.405(6) ?, α = 88.469(6)°, β = 74.892(6)°, γ = 88.256(7)°, V = 1207.5(9) ?3, Z = 1, D c = 1.731 g/cm3, μ = 2.669 mm−1, F(000) = 638, R = 0.0257, and wR = 0.0667 for 3807 observed reflections with I ≥ 2σ(I). The EuN2O6 part in the [EuIII(Cydta)(H2O)2] complex anion forms a pseudo-square antiprismatic polyhedron. The complex II is eight-coordinate as well; it is a binuclear structure that crystallizes in the monoclinic crystal system with the C 2/c space group; half of the central EuIII ion is coordinated by two nitrogen atoms from one hexadentate pdta ligand and six oxygen atoms from the same pdta ligand, one water molecule and carboxylic group from the neighboring pdta ligand respectively. The crystal data are as follows: a = 19.866(3) ?, b = 9.1017(12) ?, c = 21.010(3) ?, β = 104.972(2)°, V = 3670.1(9) ?3, Z = 8, D c = 2.046 g/cm3, μ = 3.710 mm−1, F(000) = 2240, R = 0.0213 and wR = 0.0460 for 4183 observed reflections with I ≥ 2σ(I). Otherwise, the two EuN2O6 parts in the [Eu2III(pdta)2(H2O)2]2− complex anion form a pseudo-square antiprismatic polyhedron.  相似文献   

19.
Ammonium hydrogen hexaaquacobaltate(III) isopolyvanadate [(NH4)2][Co(H2O)6] · H[V10O28] · 8H2O was synthesized and studied by X-ray diffraction, thermogravimetry, and IR and NMR spectroscopy. The crystals are triclinic, space group P [`1]\bar 1, a = 8.216(2), b = 9.965(2), c = 11.796(2) ?, α = 77.71(3)°, β = 71.11(3)°, γ = 86.11(3)°, V = 867.0(3) ?3, ρ(calcd.)= 2.501 g/cm3, Z = 1.  相似文献   

20.
The sodium hydrogen oxovanadate [Na2(H2O)8] 2H2[V10O28] · 4H2O was synthesized and studied by TGA, X-ray diffraction, and NMR and IR spectroscopy. The crystals are triclinic, space group P $ \bar 1 $ \bar 1 , a = 8.545(7) ?, b = 10.827(2) ?, c = 11.627(2) ?, α = 105.48(3)°, β = 99.38(3)°, γ = 101.29(3)°, V = 989.9(3) ?3, ρ(calcd) = 2,381 g/cm3, Z= 1.  相似文献   

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