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1.
Two novel rare earth metal coordination compounds, (MnH)4[Ho
III2
(Dtpa)2] · 12H2O (I) (Mn = methylamine, H5Dtpa = diethylenetriamine-N,N,N′,N″,N″-pentaaceticacid) and {(MnH)[HoIII(Egta)] · 3H2O}
n
(II) (H4Egta = ethyleneglycol-bis(2-aminoethylether)-N,N,N′,N′-tetraacetic acid) have been successfully synthesized through direct heating reflux and characterized by FT-IR spectroscopy, thermal analysis, and single-crystal X-ray diffraction techniques (CIF files CCDC nos. 890878 (I) and 1457061 (II)). Complex I shapes a binuclear nine-coordinate structure with distorted tricapped trigonal prismatic conformation and crystallizes in the triclinic crystal system with space group P1?. The central Ho3+ ion is coordinated by three nitrogens and six oxygens from two octadentate Dtpa ligands. The cell dimensions are as follows: a = 9.8420(10), b = 12.1319(13), c = 13.2931(15) Å, α = 89.223(2)°, β = 68.4280(10)°, γ = 72.1280(10)° and V = 1396.0(3) Å3. Complex II adopts a polynuclear nine-coordinate structure with pseudo-monocapped square antiprismatic conformation and crystallizes in the monoclinic crystal system with space group C2/c. The central Ho3+ ion is coordinated by two nitrogens and seven oxygens from two octadentate Egta ligands. The crystal data are as follows: a = 38.4755(13), b =13.5569(5), c = 8.7343(3) Å, β = 100.135(3)° and V = 4484.8(3) Å3. 相似文献
2.
Two rare-earth metal coordination compounds, (NH 4) 4[Sm III2(Httha) 2]·16H 2O ( 1) (H 6ttha?=?triethylenetetramine- N,N,N′ ,N′′ ,N′′′ ,N′′′-hexaacetic acid) and (NH 4) 4[Sm III2(dtpa) 2]·10H 2O ( 2) (H 5dtpa?=?diethylenetriamine- N,N,N′ ,N′′ ,N′′-pentaacetic acid), have been synthesized through reflux and characterized by FT -IR spectroscopy, thermal analysis, and single-crystal X-ray diffraction techniques. Sm III of (NH 4) 4[Sm III2(Httha) 2]·16H 2O ( 1) is nine-coordinate, forming tricapped trigonal prismatic coordination with three amine nitrogens and six oxygens, in which four oxygens are from one ttha and two from the other ttha. (NH 4) 4[Sm III2(Httha) 2]·16H 2O ( 1) crystallizes in the monoclinic crystal system with P2(1)/c space group. The crystal data are: a?=?13.9340(13) Å, b?=?22.890(3) Å, c?=?20.708(2) (14) Å, β?=?99.521(2)°, and V?=?6513.7(13) Å 3. There are two –NH +– groups in the [Sm III2(Httha) 2] 4?. The polymeric (NH 4) 4[Sm III2(dtpa) 2]·10H 2O ( 2) also is nine-coordinate with tricapped trigonal prismatic conformation and crystallizes in the triclinic crystal system with P–1 space group. The cell dimensions are: a?=?9.8240(8) Å, b?=?10.0329(9) Å, c?=?13.0941(11) Å, β?=?77.1640(10)°, and V?=?1227.30(18) Å 3. In (NH 4) 4[Sm III2(dtpa) 2]·10H 2O, there are two types of ammonium cations, which connect [Sm III2(dtpa) 2] 4? and lattice water through hydrogen bonds, leading to a 2-D ladder-like layer structure. 相似文献
3.
The three title complexes, NH 4[Ho III(Edta)(H 2O) 3] · 1.5H 2O (I) (H 4Edta = ethylenedianine-N,N,N′,N′-tetraacetic acid), (NH 4) 4[Ho 2 III (Dtpa) 2] · 9H 2O (II) (H 5Dtpa = diethylenetriamine-N,N,N′,N″,N″-entaacetic acid), and (NH 4) 3[Ho III(Ttha)] · 5H 2O (III) (H 6 Ttha = triethylenetetramine-N,N,N′,N″,N?,N?-hexaacetic acid), have been prepared and characterized by FT-IR, elemental analyses, and single-crystal X-ray diffraction technique. Complex I has a nine-coordinate mononuclear structure with distorted monocapped square antiprismatic conformation and its crystal structure belongs to orthorhombic system and Fdd2 space group. The crystal data are as follows: a = 19.343(9), b = 35.125(17), c = 12.364(6) Å, V = 8400(7) Å 3, Z = 16, M = 552.26, ρ calcd = 1.747 g cm ?3 μ = 3.828 mm ?1, and F(000) = 4368. Complex II has a binuclear nine-coordinate pseudomonocapped square antiprismatic conformation and its crystal structure belongs to triclinic system and space P1 group. The crystal data are as follows: a = 9.7637(16), b = 9.9722(16), c = 12.945(2) Å, α= 85.853(2)°, β = 77. 140(2)°, γ = 77.140(2)°, V = 1198.4(3) Å 3, Z = 1, M = 1340.80, ρ calcd = 1.858 g cm ?3, μ = 3.380 mm ?1, and F(000) = 674. As for complex III, it also has nine-coordinate mononuclear structure with distorted tricapped trigonal prism and its crystal structure belongs to monoclinic system and P2 1/ c space group. The crystal data are as follows: a = 10.349(3), b = 12.760(4), c = 23.142(7) Å, β = 91.020(6)°, V = 3055.6(16) Å 3, Z = 2, M = 797.55, ρ calcd = 1.734 g cm ?3, μ = 2.674 mm ?1, and F(000) = 1624. The results showed that although the ligands are different from one another in the shape and the numbers of coordination atoms, they all have nine-coordinate structures. However, one of them has binuclear structure and the other two have mononuclear structures because of the difference of the ligands. 相似文献
4.
Compounds p-HOOCC 6F 4COOH · H 2O (H 2L · H 2O), [Tb 2(H 2O) 4(L) 3 · 2H 2O] n ( I), and Tb 2(Phen) 2(L) 3 · 2H 2O ( II) are synthesized. According to the X-ray structure analysis data, the crystal structure of H 2L · H 2O is built of centrosymmetric molecules H 2L and molecules of water of crystallization. The crystal structure of compound I is built of layers of coordination 2D polymer [Tb 2(H 2O) 4(L) 3] n and molecules of water of crystallization. The ligands are the L 2? anions performing both the tetradentate bridging and pentadentate bridging-chelating functions. The coordination polyhedron TbO 9 is a distorted three-capped trigonal prism. Acid H 2L manifests photoluminescence in the UV region (?? max = 368 nm). Compounds I and II have the green luminescence characteristic of the Tb 3+ ions, and the band with ?? max = 545 nm (transition 5 D 4?? 7 F 5) is maximum in intensity. The photoluminescence intensity of compound II is higher than that for compound I. 相似文献
5.
Two Cu(II) hydroxo succinates [Cu 3(H 2O) 2(OH) 2(C 4H 4O 4) 2]?·?4H 2O ( 1) and [Cu 4(H 2O) 2(OH) 4(C 4H 4O 4) 2]?·?5H 2O ( 2) and one Cu(II) hydroxo glutarate [Cu 5(OH) 6(C 5H 6O 4) 2]?·?4H 2O ( 3) have been prepared and structurally characterized by single crystal X-ray diffraction methods. They feature 1D and 2D copper oxygen connectivity of elongated {CuO 6} octahedra in “4?+?1?+?1” and “4?+?2” coordination geometries. Within 1, linear trimers of three edge-sharing {CuO 6} octahedra are connected into copper oxygen chains, which are bridged by the anti conformational succinate anions to generate 2D layers with mono terminally coordinating gauche succinate anions on both sides. The layers are assembled into a 3D framework by interlayer hydrogen bonds with lattice H 2O molecules distributed in channels. Different from 1, the principal building units in 2 are linear tetramers of four edge-sharing {CuO 6} octahedra. The tetramers are condensed into copper oxygen chains and the succinate anions interlink them into a 3D framework with triangular channels filled by lattice H 2O molecules. The {CuO 6} octahedra in 3 are edge-shared to form unprecedented 2D inorganic layers with mono terminally coordinating glutarate anions on both sides. Interlayer hydrogen bonding interactions are responsible for supramolecular assembly of the layers into a 3D framework with lattice H 2O molecules in the channels. The inorganic layers in 3 can be described as hexagonal close packing of oxygen atoms with the Cu atoms in the octahedral cavities. The title compounds were further characterized by elemental analyses, IR spectra and thermal analyses. 相似文献
6.
Two title complexes, [Tb III(Eg3a)(H 2O) 2] · 4.5H 2O ( I) (H 3Eg3a = 3-carboxymethyl-6, 9-dioxa-3,12-diazatetradecanedioic acid) and K[Tb III(Edta)(H 2O) 3] · 5H 2O( II) (H 4Edta = ethylenediamine-N,N,N′,N′-tetraaceti acid), were prepared and characterized by FT-IR, elemental analyses, TGA-DTA-DTG, and single-crystal X-ray diffraction technique. For I, the Tb 3+ ion is nine-coordinated by an Eg3a ligand and two coordination water molecules, yielding a monocapped square-antiprismatic (MCSAP) conformation. Complex I crystallizes in the monoclinic system with P2 1/ c space group. The crystal data are as follows: a = 9.237(3), b = 10.018(3), c = 23.580(7) Å, β = 99.021(5)°, V = 2155.2(11) Å 3, Z = 4, ρ = 1.822 Mg m ?3, μ = 3.353 mm ?1, F(000) = 1180, R 1 = 0.0445 and wR 2 = 0.1034 for 4262 observed reflections with I ≥ 2σ( I). For II, the Tb 3+ ion is nine-coordinated by an Edta ligand and three coordinate water molecules also yielding a MCSAP conformation. Complex II crystallizes in the orthorhombic system with Fdd2 space group. The crystal data are as follows: a = 19.373(5), b = 35.429(10), c = 12.114(3) Å, V = 8315(4) Å 3, Z = 16, ρ = 2.014 Mg m ?3, μ = 2.014 mm ?1, F(000) = 5024, R 1 = 0.0224 and wR 2 = 0.0557 for 3189 observed reflections with I ≥ 2σ( I). The potassium cations bridge the coordination spheres yielding many infinite long 1-D zigzag-type chains. The molecular structure of I is more stable than that of II. According to thermal analyses, the collapsing temperatures of crystal structure are 314°C for I and 348°C for II, which indicates that the crystal structure of II is more stable. 相似文献
7.
The title complex [Cu(tssb)2]·2[(H3O)Cl]·4H2O (C18H34Cl2CuN2O14S2) (tssb = taurine salicylaldehyde Schiff base) has been synthesized by the reaction of taurine salicylaldehyde Schiff base (tssb) and copper acetate in water-ethanol. Its single-crystal structure was determined by X-ray diffraction method. The crystal structure belongs to triclinic, space group P with a = 0.7407(1), b = 1.3329(3), c = 1.5736(3)nm, α = 103.800(4), β = 95.030(4), γ = 104.416(4)°, Mr = 701.06, V = 1.4433(5) nm3, Z = 2, Dc = 1.613 g/cm3, μ = 1.153 mm-1 and F(000) = 726. The compound is an infinitely expanding three-dimensional network connected with hydrogen bonds. The Cu(Ⅱ) atom is coordinated by two nitrogen and two oxygen atoms to form a distorted planar coordination compound which adopts anti-configuration because two sulfonic acid groups are positioned diagonally on a plane. 相似文献
8.
Two lanthanide complexes, (mnH) 2[Eu III(egta)] 2·6H 2O ( 1) (H 4egta = ethyleneglycol-bis-(2aminoethylether)- N,N,N′ ,N′-tetraacetic acid) and (mnH) 4[Eu III2(dtpa) 2]·6H 2O ( 2) (H 5dtpa = diethylenetriamine- N,N,N′ ,N″,N″-pentaacetic acid), have been synthesized and characterized by FT -IR spectroscopy, thermal analysis, and single-crystal X-ray diffraction. X-ray diffraction reveals that 1 is multinuclear nine-coordinate and crystallizes in the monoclinic crystal system with space group C2/c. The obtained cell dimensions are a = 38.513(3)?Å, b = 13.5877(8)?Å, c = 8.7051(5)?Å, β = 99.6780(10)°, and 4490.6(5)?Å 3. Each methylamine (mnH +) cation in 1, through hydrogen bonds, connects three adjacent [Eu III(egta)] ? anions. The [Eu III(egta)] ? anions connect one another forming a 1-D multinuclear zigzag chain structure along the c-axis. Complex 2 is nine-coordinate binuclear structure with tricapped trigonal prismatic conformation and crystallizing in the monoclinic crystal system, but with space group P21/n. The obtained cell dimensions are a = 9.9132(8)?Å, b = 24.1027(18)?Å, c = 10.7120(10)?Å, β = 109.1220(10)°, and 2418.2(3)?Å 3. For 2, there are two kinds of methylamine cations (mnH +) connecting [Eu III2(dtpa) 2] 4? complex anions and lattice waters through hydrogen bonds, leading to formation of a 2-D ladder-like layer structure. 相似文献
9.
The binuclear complexes [Cu 2L 2(H 2O) 4] · 5H 2O ( 1) and [Ni 2L 2(H 2O) 4] · 2H 2O ( 2) (where L = C 11H 11NO 5S, H 2 L = 2-[(3-formyl-5-methyl-2-hydroxy-benzylidene)-amino]ethanesulfonic acid) have been synthesized and characterized by IR, elemental analysis and X-ray diffraction. The crystals belong to the monoclinic system, space group P2 1/ c. Complex 1: a = 16.8902(12), b = 11.2829(6), c = 17.4249(11) Å; β = 106.709(4)°; S = 1.131; V = 3180.5(3) Å 3; Z = 4; D Calcd = 1.729 g cm ?3; F(000) = 1712; μ = 1.554 mm ?1; R 1 = 0.0519, wR 2 = 0.1349; complex 2: a = 11.399(2), b = 19.985(3), c = 7.3694(10) Å; β = 108.664(7)°; S = 1.157; V = 1590.6(4) Å 3; Z = 2; D Calcd = 1.604 g cm ?3; F(000) = 800; μ = 1.388 mm ?1; R 1 = 0.1859, wR 2 = 0.4346. The geometry around each metal(II) center can be described as slightly distorted octahedral. Water-sulfonic clusters and (H 2O) 4 water clusters can be observed for 1 from the crystal packing diagram, while cavity and offset face-to-face π–π stacking can be observed for 2. The complexes have been tested for the antibacterial activities which show antibacterial activities of 1 for β-hemolytic streptococcus, Staphylococcus aureus and Escherichia coli, and the antibacterial activity of 2 only for β-hemolytic streptococcus. 相似文献
10.
Three complexes, Na 4[Dy III(dtpa)(H 2O)] 2?·?16H 2O, Na[Dy III(edta)(H 2O) 3]?·?3.25H 2O and Na 3[Dy III (nta) 2(H 2O)]?·?5.5H 2O, have been synthesized in aqueous solution and characterized by FT–IR, elemental analyses, TG–DTA and single-crystal X-ray diffraction. Na 4[Dy III(dtpa)(H 2O)] 2?·?16H 2O crystallizes in the monoclinic system with P2 1/ n space group, a?=?18.158(10)?Å, b?=?14.968(9)?Å, c?=?20.769(12)?Å, β?=?108.552(9)°, V?=?5351(5)?Å 3, Z?=?4, M?=?1517.87?g?mol ?1, D c?=?1.879?g?cm ?3, μ?=?2.914?mm ?1, F(000)?=?3032, and its structure is refined to R 1( F)?=?0.0500 for 9384 observed reflections [ I?>?2σ( I)]. Na[Dy III(edta)(H 2O) 3]?·?3.25H 2O crystallizes in the orthorhombic system with Fdd2 space group, a?=?19.338(7)?Å, b?=?35.378(13)?Å, c?=?12.137(5)?Å, β?=?90°, V?=?8303(5)?Å 3, Z?=?16, M?=?586.31?g?mol ?1, D c?=?1.876?g?cm ?3, μ?=?3.690?mm ?1, F(000)?=?4632, and its structure is refined to R 1( F)?=?0.0307 for 4027 observed reflections [ I?>?2σ( I)]. Na 3[Dy III(nta) 2(H 2O)]?·?5.5H 2O crystallizes in the orthorhombic system with Pccn space group, a?=?15.964(12)?Å, b?=?19.665(15)?Å, c?=?14.552(11)?Å, β?=?90°, V?=?4568(6)?Å 3, Z?=?8, M?=?724.81?g?mol ?1, D c?=?2.102?g?cm ?3, μ?=?3.422?mm ?1, F(000)?=?2848, and its structure is refined to R 1( F)?=?0.0449 for 4033 observed reflections [ I?>?2?σ( I)]. The coordination polyhedra are tricapped trigonal prism for Na 4[Dy III(dtpa)(H 2O)] 2?·?16H 2O and Na 3[Dy III(nta) 2(H 2O)]?·?5.5H 2O, but monocapped square antiprism for Na[Dy III(edta)(H 2O) 3]?·?3.25H 2O. The crystal structures of these three complexes are completely different from one another. The three-dimensional geometries of three polymers are 3-D layer-shaped structure for Na 4[Dy III(dtpa)(H 2O)] 2?·?16H 2O, 1-D zigzag type structure for Na[Dy III(edta)(H 2O) 3]?·?3.25H 2O and a 2-D parallelogram for Na 3[Dy III(nta) 2(H 2O)]?·?5.5H 2O. According to thermal analyses, the collapsing temperatures are 356°C for Na 4[Dy III(dtpa)(H 2O)] 2?·?16H 2O, 371°C for Na[Dy III(edta)(H 2O) 3]?·?3.25H 2O and 387°C for Na 3[Dy III(nta) 2(H 2O)]?·?5.5H 2O, which indicates that their crystal structures are very stable. 相似文献
12.
The title complexes, Na[Er III(Cydta)(H 2O) 2] · 5H 2O ( I) and Na 2[Sm III(Cydta)][Sm III(Cydta)(H 2O) 3] · 11H 2O ( II) (Cydta is trans-1,2-cyclohexanediaminetetraacetic acid), are prepared and characterized using IR, elemental analyses, and single-crystal X-ray diffraction techniques. Crystal I belongs to triclinic system (space group P1), which has a mononuclear eight-coordinate slightly distorted square antiprismatic conformation. The crystal data are as follows: a = 8.371(12) Å, b = 9.952(14) Å, c = 14.74(2) Å, α = 88.32(2)°, β = 76.30(2)°, γ = 87.87(2)°, V = 1192(3) Å 3, Z = 1, ρ = 1.835 g/cm 3, μ = 3.612 mm ?1, F(000) = 658, R = 0.0194, and wR = 0.0520 for 4130 observed reflections with I≥2σ( I). Crystal II belongs to monoclinic system (space group P2 1/ n), which has the binuclear nine-coordinate structure with tricapped trigonal prismatic conformation for Sm(1) and the pseudomonocapped square antiprismatic conformation for Sm(2). The crystal data are as follows: a = 12.283(6) Å, b = 15.626(7) Å, c = 25.875(12) Å, β = 97.962(7)°, V = 4919(4) Å 3, Z = 4, ρ = 1.717 g/cm 3, μ = 2.476 mm ?1, F(000) = 2536, R = 0.0781, and wR = 0.1745 for 8554 observed reflections with I ≥ 2σ( I). 相似文献
13.
The compounds (NH 4) 6[Mo 6V 2O 24(C 2O 4) 2]·6H 2O ( I) and (NH 4) 4[H 2Mo 2V 2O 12(C 2O 4) 2]·2H 2O ( II) have been prepared from molybdenum(VI) oxide and ammonium vanadate in aqueous solution through the addition of ammonium oxalate, and their structures determined by X-ray structure analysis. Whereas the molybdovanadate anion [Mo 6V 2O 24(C 2O 4) 2] 6− found in ( I) consists of six MoO 6 and two VO 6 edge-sharing octahedra of the γ-[Mo 8O 26] 4− type structure, the tetranuclear anion [H 2Mo 2V 2O 12(C 2O 4) 2] 4− of ( II) adopts the structure with a M 4O 16 core. Both complexes contain bidentate oxalato ligands bonded to the vanadium ions. In both crystal structures the molybdovanadate anions are mutually hydrogen bonded by ammonium ions and water molecules. 相似文献
14.
Two new bimetallic cyano-bridged complexes [Ce(DMSO)4(H2O)3Fe(CN)6]·H2O 1 and [La(DMSO)4(H2O)3Co(CN)6]·H2O 2 have been prepared by the ball milling reaction method and structurally characterized by X-ray single-crystal structure analyses. Crystallographic data for 1:C14H32CeFeN6O8S4, Mr = 736.67, monoclinic, space group P21/n, a = 14.952(1), b =13.7276(9), c = 15.392(1) (A), β = 108.288(1)°, V = 2999.6(4) (A)3, Z = 4, Dc= 1.631 g/cm3,μ =2.304 mm-1, F(000) = 1480, R = 0.0593 and wR = 0.1611; and those for 2: C14H32CoLaN6O8S4,Mr=738.54, monoclinic, space group P21/n, a = 14.945(3), b = 13.731(3), c = 15.300(3) (A), β=107.806(1)°, V= 2989.3(11) (A)3, Z = 4, Dc = 1.641 g/cm3,μ = 2.288 mm-1, F(000) = 1480, R =0.0383 and wR = 0.1132. In both complexes the lanthanide ion is eight-coordinated in a square antiprism arrangement, and the Fe(Ⅲ) or Co(Ⅲ) ion in a nearly regular octahedral environment.The [LnM(CN)6(DMSO)4(H2O)3]·H2O (Ln = Ce and M = Fe for 1; Ln = La and M = Co for 2)species are held together via hydrogen bonds by coordinated water molecules, lattice water molecules and nitrogen atoms of cyanide groups to form a three-dimensional framework. 相似文献
15.
Cs 2[(UO 2) 2(C 2O 4) 3] ( I) and Cs 2[UO 2(C 3H 2O 4) 2] · H 2O ( II) have been synthesized and studied by X-ray diffraction. The crystals of complexes I and II are monoclinic: a = 8.1453(2) Å, b = 8.9831(2) Å, c = 11.3897(4) Å, β = 104.0950(10)°, V = 808.29(4) Å 3, space group P2 1/ n, Z = 2, and R 1 = 0.0255 for I and a = 9.6998(2) Å, b = 17.8686(3) Å, c = 8.2074(2) Å, β = 97.5780(10)°, V = 1410.10(5) Å 3, space group P2 1/ c, Z = 4, and R 1 = 0.0287 for II. The uranium-containing structural units of complexes I and II are [(UO 2) 2(C 2O 4) 3] 2? chains and [UO 2(C 3H 2O 4) 2] 2 4? dimers, which belong to the AK 0.5 02 T 11 and AT 11B 01 crystallochemical groups (A = UO 2 2+ , K 02 and T 11 = C 2O 4 2? , T 11 and B 01 = C 3H 2O 4 2? ) of uranyl complexes. 相似文献
16.
Reaction of a freshly prepared Ni(OH) 2?2 x (CO 3) x · yH 2O with maleic acid in H 2O at room temperature afforded [Ni(H 2O) 6][Ni(H 2O) 2(C 4H 2O 4)]·4H 2O, which consists of [Ni(H 2O) 6] 2+ cations, [Ni(H 2O) 2(C 4H 2O 4)] 2? anions and lattice H 2O molecules. Ni atoms in cations are octahedrally coordinated and Ni atoms in anions are each octahedrally coordinated by bidentate chelating maleato ligands and two water molecules at trans positions. Cations and anions are interlinked by hydrogen bonds to form 1D chains, which are hexagonally arranged and connected by the lattice water molecules. When heated in a flowing argon stream, the compound decomposes, with complete dehydration being followed by dissociation of nickel maleate into NiO and maleic anhydride. 相似文献
17.
Reactions of ZrOCl 2·8H 2O in aqueous solution with a carboxylic acid in the presence of K 2CO 3 have been studied as a route to Zr IV-carboxylates. With malonic acid (HO 2CCH 2CO 2H) (H 2mal) the product has been identified as K 4[Zr(mal) 4]·2H 2O (1) by X-ray crystallography. The individual eight-coordinate zirconium anions contain four bidentate (OO) malonate anions with the metal geometry approximating to a square antiprism with each chelating ligand spanning the two square faces, Zr—O 2.091(3)–2.288(3) Å. The four potassium cations feature irregular coordination spheres of oxygen atoms [from both H 2O and (mal) ligand molecules] with a 7–9 coordination range. With 2,6-dicarboxypicolinicacid (HO 2CC 5NH 3CO 2H) (H 2dipic) the product has been characterised as K 4[Zr(dipic) 3] 2·13.5H 2O (2) following X-ray diffraction studies. The structure consists of two [Zr(dipic) 3] 2- anions, four potassium cations and lattice solvate (H 2O) molecules. Individual anions feature nine-coordinate zirconium in which each dipic ligand is terdentate, being bonded via one N (pyridine) and two O (carboxylate) atoms. The metal geometry approximates to tricapped trigonal prismatic with each nitrogen atom capping a regular face of four oxygen atoms, Zr—O, 2.216(6)–2.261(6) Å; Zr—N, 2.343(8)–2.361(7) Å. The potassium cations show similar environments to those observed in structure (1). Dehydration of ZrOCl 2·8H 2O using SOCl 2 in the presence of an excess of THF effects removal of coordinated H 2O molecules and hydroxy bridging groups to provide the anhydrous bis-adduct ZrCl 4(thf) 2 in good yield (72%). 相似文献
18.
The molecular and crystal structure of the title complex (I) obtained by addition of tin fluoride in a hydrofluoric acid solution to 18-crown-6 in methanol was investigated by X-ray structure analysis. The crystals are monoclinic, space group P2 1/n, a = 13.497(3), b = 7.806(2), c = 9.892(2) Å, β = 95.57(3)°, Z = 2 for C 12H 32F 4O 10Sn. In the polymer chain, the crown ether molecules alternate with the inorganic complexes [trans-SnF 4(H 2O) 2] and are linked to them by O-H...O type hydrogen bonds involving the intermediate water molecules. The weak C-H...F interactions bind the chains into the layers which are parallel to the xz plane. 相似文献
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