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1.
Double ionic complexes [M(C5H5NCOO)3(H2O)2][Cr(NCS)6] · nH2O, where M = Eu (I), n = 1.15; Dy (II), Er (III), n = 1.5; M = Yb (IV), n = 2, have been synthesized by the reaction between M(NO3)3, M = Eu, Dy, Er, Yb, K3[Cr(NCS)6], and nicotinic acid (C5H5NCOO) in an aqueous solution and studied by chemical analysis, IR spectroscopy, and X-ray diffraction. Crystals of complexes IIV are monoclinic, space group P21/n, Z = 4; a = 9.5358(2) Å, b = 25.4871(5) Å, c = 15.4303(4) Å, β = 105.513(1)°, V = 3613.6(1) Å3, ρcalcd = 1.799 g/cm3 for I, a = 9.5901(5) Å, b = 25.8599(15) Å, c = 15.6316(9) Å, β = 106.829(2)°, V = 3710.6(4) Å3, ρcalcd = 1.782 g/cm3 for II, a = 9.5640(3) Å, b = 25.8936(11) Å, c = 15.6498(7) Å, β = 106.895(2)°, V = 3708.3(3) Å3, ρcalcd = 1.791 g/cm3 for III, and a = 9.5049(2) Å, b = 25.6378(4) Å, c = 15.5120(3) Å, β = 106.934(1)°, V = 3616.1(1) Å3, ρcalcd = 1.864 g/cm3 for IV.  相似文献   

2.
Novel complex salts [Au(en)2]Cl(ReO4)2 (I) and [Au(en)2](ReO4)3 (II), en = ethylenediamine, are obtained. Their crystal structures are determined by single crystal X-ray diffraction. Complex I crystallizes in the triclinic crystal system: a = 6.2172(7) Å, b = 7.1644(8) Å, c = 8.8829(8) Å, α = 96.605(4)°, β = 110.000(4)°, γ = 97.802(4)°, P-1 space group, Z = 1, d x = 3.905 g/cm3; complex II crystallizes in the monoclinic crystal system: a = 15.244(2) Å, b = 7.6809(8) Å, c = 9.3476(12) Å, β = 127.004(3)°, C2 space group, Z = 4, d x = 4.057 g/cm3.  相似文献   

3.
The structures of the Pd4(SBu)4(OAc)4 (I) and Pd6 (SBu)12 (II) palladium clusters are determined by the X-ray diffraction method. For cluster I: a = 8.650(2), b = 12.314(2), c = 17.659(4) Å, α = 78.03(3)°, β = 86.71(2)°, γ = 78.13(3)°, V = 1800.8(7) Å3, ρcalcd = 1.878 g/cm3, space group P \(\bar 1\), Z = 4, N = 3403, R = 0.0468; for structure II: a = 10.748(2), b = 12.840(3), c = 15.233(3) Å, α = 65.31(3)°, β = 70.10(3)°, γ = 72.91(3)°, V = 1767.4(6) Å3, ρ calcd = 1.605 g/cm3, space group P \(\bar 1\), Z = 1, N = 3498, R = 0.0729. In cluster I, four Pd atoms form a planar cycle. The neighboring Pd atoms are bound by two acetate or two mercaptide bridges (Pd…Pd 2.95–3.23 Å, Pd…Pd angles 87.15°–92.85°). In cluster II, the Pd atoms form a planar six-membered cycle with Pd···Pd distances of 3.09–3.14 Å, the PdPdPd angles being 118.95°–120.80°. The Pd atoms are linked in pairs by two mercaptide bridges. The formation of clusters I and II in solution is proved by IR spectroscopy and calorimetry. Analogous clusters are formed in solution upon the reaction of palladium(II) diacetate with thiophenol.  相似文献   

4.
Zinc(II) and manganese(II) complexes of 2-(diphenylacetyl)indandione-1,3 (HL) were synthesized. Crystals of [M(DMSO)2L2] · CHCl3, where M= Zn(II) (I) and Mn(II) (II), obtained from chloroform plus dimethyl sulfoxide (DMSO) mixture were found to be isostructural based on the similarity of their unit cell parameters and unit cell volumes. The crystals are triclinic, Z = 2, space group P \(\bar 1\); a = 10.422(1) Å, b = 11.929(1) Å, c = 20.429(1) Å, α = 73.616(1)°, β = 85.095(1)°, γ = 77.586(1)° for complex I; a = 10.436(1) Å, b = 12.297(1) Å, c = 19.924(2) Å, α = 78.138(2)°, β = 87.625(2)°, γ = 82.048(2)° for complex II. X-ray structural analysis of complex I was carried out. For complex II, the structure was not refined because all of its atoms are each disordered over three to five positions. The two DMSO molecules in complex I coordinate the central metal atoms in the monodentate mode via their donor oxygen atoms to occupy an axial position and an equatorial position in an octahedral polyhedron. The other four positions are occupied by the four oxygen atoms of the two deprotonated ligands L? coordinated in the bidentate-cyclic mode. The outer sphere of complex I contains the solvating chloroform molecule.  相似文献   

5.
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   

6.
Compounds Y2SiO4Q (Q = S, Se) are obtained by the interaction of oxides and elemental substances in cesium chloride flux. The structures of these compounds are determined by the single crystal XRD analysis. These compounds isostructural and crystallize in the space group Pbcm with the following parameters: Y2SiO4S (I) a = 6.0462(8) Å, b = 6.8976(9) Å, c = 10.6558(13) Å, V = 444.39(10) Å3; Y2SiO4Se (II) a = 5.9935(7) Å, b = 6.9216(8) Å, c = 10.7688(12) Å, V = 446.74(9) Å3. The measured fluxing points are 1650±15 °С for I and 1850±15 °С for II.  相似文献   

7.
Two new oxovanadium(V) complexes, [VOL1(OCH3)(CH3OH)] (I) and [VOL2(OCH3)] (II), where L1 and L2 are the di-anionic form of N'-[1-(5-fluoro-2-hydroxyphenyl)methylidene]nicotinohydrazide and N'-(5-fluoro-2-hydroxybenzylidene)-2-hydroxynaphthylhydrazide, respectively, have been synthesized and characterized by elemental analysis, FT-IR spectra, and single crystal X-ray determination (CIF files CCDC nos. 891852 (I), 891853 (II)). The crystal of I is monoclinic: space group P21/c, a = 8.061(1), b = 15.293(2), c = 13.471(2) Å, ß = 92.595(2)°, V = 1658.8(4) Å3, Z = 4. The crystal of II is monoclinic: space group P21/n, a = 7.4454(9), b = 8.0833(9), c = 28.906(2) Å, ß = 92.644(2)°, V = 1737.8(3) Å3, Z = 4. The V atom in I is in an octahedral coordination, and that in II is in a square-pyramidal coordination. The antibacterial activity of the compounds against various bacteria was assayed.  相似文献   

8.
Compound [VO(acac)2] reacts with the Schiff bases N′-(5-bromo-2-hydroxybenzylidene)-2-hydroxy-3-methylbenzohydrazide (H2Bhm) and 4-bromo-2-[(2-piperidin-1-ylethylimino)methyl]phenol (HBpp) in absolute methanol to give the oxovanadium(V) complexes [VO(Bhm)(OCH3)(CH3OH)] (I) and [VO2(Bpp)] (II), respectively. Both complexes were characterized by elemental analysis, IR spectra, and single-crystal X-ray determination. The crystal of I crystallizes in the triclinic space group \(P\bar 1\) with a = 7.625(2), b = 11.240(3), c = 12.156(4) Å, α = 77.404(5)°, β = 75.770(4)°, γ = 79.922(5)°, V = 977.4(5) Å3, Z = 2. The crystal of II crystallizes in the monoclinic space group P2/c with a = 26.760(3), b = 6.655(1), c = 17.570(2) Å, β = 100.335(2)°, V = 3078.2(7) Å3, Z = 8. The V atom in I is in an octahedral coordination, and those in II are intervenient between square pyramidal and trigonal bipyramidal coordination.  相似文献   

9.
A new mononuclear cobalt(III) complex, [CoL2(N3)]2 · CH3OH (I), and a new mononuclear zinc(II) complex, [ZnLCl(CH3OH)] (II) (HL = 4-chloro-2-[(2-morpholin-4-ylethylimino)methyl]phenol), were prepared and structurally characterized by elemental analyses, infrared spectroscopy, and single- crystal X-ray diffraction. The crystal of I is monoclinic: space group P21/c, a = 18.742(2) Å, b = 15.197(2) Å, c = 25.646(2) Å, β = 125.996(3)°, V = 5909.8(11) Å3, Z = 4. The crystal of II is monoclinic: space group P21/c, a = 7.257(1) Å, b = 24.707(2) Å, c = 9.637(1) Å, β = 101.557(2)°, V = 1692.9(3) Å3, Z = 4. The Co atom in I is in an octahedral coordination, and the Zn atom in II is in a trigonal-bipyramidal coordination. The urease inhibitory test shows that complex I has strong urease inhibitory activity, while complex II has no activity.  相似文献   

10.
The synthesis, vibrational spectra, and X-ray diffraction analysis results for 2-(diphenylphosphinylmethoxy) aniline, 2-[(C6H5)2P(O)OCH2]C6H4NH2(I), are described. The crystals are monoclinic: a = 18.4515(17) Å, b = 10.5421(12) Å, c = 17.897(2) Å, β = 104.479(8)°, V = 3370.7(6) Å3, Z = 8, space group P21/c, R = 0.0546 for 1770 reflections with I > 2σ(I). The unit cell contains two crystallographically independent molecules Ia and Ib joined by an N-H …O hydrogen bond between a hydrogen atom of the amino group of aniline in molecule Ia (Ib) and the phosphoryl oxygen atom of molecule Ib (Ia) (O…H 2.18 and 2.19 Å, N…O, 2.979(5) and 3.000(5) Å; NHO angle, 154° and 157°).  相似文献   

11.
Two ethylenediamine derivatives—N-(2-ammoniumethyl)carbamate HN(COO?)CH2CH2N+H3 (I) and tetraacetylethylenediamine (H3CC(O))2NCH2CH2N(C(O)CH3)2 (II) (synthesized for the first time)—have been synthesized and characterized by X-ray crystallography. Compounds I and II are isolated as minor admixtures upon an attempt to synthesize ethylenediamine complexes of lanthanum and neodymium nitrates, respectively. The crystals of I and II are monoclinic: a = 7.778 Å, b = 8.060 Å, c = 7.568 Å, β = 95.73°, Z = 4, space group P21/c (I); a = 5.946, b = 10.255, c = 9.343 Å, β = 95.72°, Z = 2, space group P21/c (II). The bond lengths and bond angles lie within the corresponding standard values. Compounds I and II have different conformations of the N-C-C-N ethylenediamine moiety: gauche in I and trans in II, and the corresponding torsion angles are equal to 66.6° and 180°, respectively.  相似文献   

12.
The tetranuclear cluster rhenium complexes Cs3H[Re4Q4Cl12] · 3.33H2O (Q = Te (I) and Se (II)) with the Cl atoms as terminal ligands were obtained and structurally characterized. The structures of complexes I and II were determined by X-ray diffraction analysis. Their isostructural crystals are monoclinic; space group C2, Z = 6; a = 26.403(8) Å, b = 16.495(5) Å, c = 11.744(3) Å, β = 91.25(2)°, V = 5113(2) Å3 (I); a = 26.573(3) Å, b = 16.461(3) Å, c = 11.726(2) Å, β = 91.381(4)°, V = 5127.6(14) Å3 (II).  相似文献   

13.
Heteroligand complexes [Co2(HMTA)(iso-Bu2PS2)4] (I) (μeff = 4.67 μB) and [Cd2(HMTA)(iso-Bu2PS2)4] (II) have been synthesized. Single crystals of compounds I and II have been obtained. The crystals are monoclinic: a = 32.622(2) Å, b = 9.4891(6) Å, c = 21.7570(13) Å, β = 125.774(1)o, V = 5464.3(6) Å,3, Z = 4, ρcalcd = 1.331 g/cm3 for I; a = 34.6092(7) Å, b = 9.5595(2) Å, c = 22.3473(5) Å, β = 127.144(1)o, V = 5893.5(2) Å, Z = 4, ρcalcd = 1.355 g/cm3 for II; space group for both complexes C2/c. Structures I and II are based on discrete binuclear molecules. The coordination polyhedra of the Co and Cd atoms are distorted tetragonal pyramids NS4, with the bases formed by four S atoms of two bidentate chelating ligand iso-Bu2PS 2 ? and the axial vertices occupied by N atoms of bidentate bridging HMTA ligand. The character of interaction of the molecules in structures I and II is considered.  相似文献   

14.
Two new dioxomolybdenum(VI) complexes, [MoO2L1(MeOH)] (I) and [MoO2L2] (II), where L1 and L2 are the anionic forms of N'-(2-hydroxy-3,5-di-tert-butylbenzylidene)-4-methoxybenzohydrazide and 2-amino-N'-(2-hydroxy-3,5-di-tert-butylbenzylidene)benzohydrazide, respectively, have been synthesized and characterized by elemental analysis, FT-IR spectra, and single crystal X-ray determination (CF files CCDC nos. 1448089 (I), 1487063 (II)). The crystal of I is monoclinic: space group P21/n, a = 7.353(1), b = 24.758(3), c = 13.891(2) Å, β = 101.013(2)°, V = 2482.3(6) Å3, Z = 4, R 1 = 0.0848, wR 2 = 0.2050. The crystal of II is monoclinic: space group P21/c, a = 6.752(1), b = 16.947(1), c = 19.510(1) Å, β = 96.891(2)°, V = 2216.5(4) Å3, Z = 4, R 1 = 0.0670, wR 2 = 0.1638. The Mo atom in complex I is in octahedral coordination, with three donor atoms of the hydrazone ligand, two oxo groups, and one methanol O atom. The Mo atom in complex II is in square pyramidal coordination, with three donor atoms of the hydrazone ligand, and two oxo groups. The complexes have interesting catalytic properties for sulfoxidation reactions.  相似文献   

15.
New double complexes [Co(DMSO)6][SiF6] ? 2H2O (I) and [Co(DMF)3(H2O)3][SiF6] ? DMF (II) have been synthesized and studied by IR spectroscopy and X-ray diffraction. Crystals of complex I belong to the tetragonal symmetry system, space group R3?, Z = 3, a = 11.8232(3) Å, c = 18.4699(5) Å, V = 2235.97(10) Å3, ρcalc = 1.573 g/cm3. Crystals of complex II are triclinic, space group P1?, Z = 2, a = 8.6264(4) Å, b = 10.1419(4) Å, c = 13.9657(6) Å, α = 100.847(2)°, β = 98.549(2)°, γ = 93.479(2)°, V = 1181.71(9) Å3, ρcalc = 1.539 g/cm3.  相似文献   

16.
Dichloro(ethylenediamine-N,N-di-3-propionato)zinc (I) has been synthesized for the first time by the reaction between acrylic acid and ethylenediamine coordinated with ZnCl2 in an aqueous medium. Complex I has been characterized by IR, Raman, and 1H,13C NMR spectroscopy, mass spectrometry, and elemental analysis. The X-ray diffraction analysis of complex I has also been performed. Crystals are monoclinic, а = 9.7792(4) Å, b = 9.9805(4) Å, c = 13.1130(5) Å, β = 101.5620(10)°, space group Р21/c, Z = 4, V = 1253.88(9) Å3, ρcalc = 1.804 g/cm3. The coordination polyhedra of Zn atoms in complex I are slightly distorted {ZnCl2O2} tetrahedra, each of which are built of two chlorine atoms and the carboxyl oxygen atoms of the two propionic groups of two ligand molecules and form a polymeric layer parallel to crystallographic plant (100). Bond lengths are Zn–О 1.970(1) and 1.976(1); Zn–Cl 2.2600(4) and 2.2693(4) Å. The ligand molecule in complex I has a double betaine structure.  相似文献   

17.
Crystals of double polyphosphates EuCs5(PO3)8 (I) and GdCs5(PO3)8 (II) have been studied by X-ray diffraction. The isostructural crystals of I and II are monoclinic, space group C2. Only unit cell parameters have been determined for the crystals of double Pr and Cs polyphosphate (III). This crystal is isostructural with earlier studied La3Cs15P24O72 · 6H2O (IV). The crystals of compounds III and IV are triclinic, space group P1, Z = 1; a = 11.987(2) and 12.178(5) Å, b = 14.754(8) and 14.740(8) Å, c = 14.692(8) and 14.847(9) Å, α = 60.15(4)° and 60.87(5)°, β = 67.04(4)° and 66.35(4)°, γ = 78.76(3)° and 77.54(4)°, respectively. In compounds I and II, the polyphosphate anions exist as infinite chains. The MIIIO8 polyhedra are isolated from each other but share edges and faces with the CsO n polyhedra.  相似文献   

18.
Two new complexes were synthesized, namely, 7: 2 (2.2.2-cryptand)potassium chloride and (2.2.2-cryptand)ammonium bromide(0.75)chloride(0.25) hydrates: [M(Crypt-222)]+ · Hal? · 3.5H2O, where M = K, Hal = Cl (I) and M = NH4, Hal = Br0.75Cl0.25 (II). The structures of two isomorphous crystals were studied by X-ray diffraction analysis. Trigonal (space group P \(\bar 3\), Z = 2) structures I (a = 11.763 Å, c = 11.262 Å) and II (a = 11.945 Å, c = 11.337 Å) were solved by direct methods and refined by the full-matrix least-squares method in the anisotropic approximation to R = 0.057 (I) and 0.065 (II) for all 2626 (I) and 1654 (II) independent measured reflections (CAD-4 automated diffractometer, λMoK α). In structures I and II, the host-guest [M(Crypt-222)]+ complex cation lies on the threefold crystallographic axis and has the approximate D 3 symmetry. In complex I, the coordination polyhedron of the K+ cation (CN = 8) is a bicapped trigonal prism somewhat distorted toward an antiprism. Complexes I and II contain H-bonded disordered cubes of the water molecules and the Cl? or Br? anions.  相似文献   

19.
The structures of three novel octahedral rhenium cluster compounds [Re6S8(CN)2(py)4]·H2O (1), [Re6S8(CN)2(4-Mepy)4] (2), [Re6S8(CN)2(4-Mepy)4]·4-Mepy (3) (py = pyridine, 4-Mepy = 4-methylpyridine) are determined by X-ray crystallography. Crystal data are: C2/m space group, a = 14.813(1) Å, b = 14.772(1) Å, c = 9.2122(6) Å, β = 119.085(2)°, V = 1761.7(2) Å3, d x = 3.318 g/cm3, R = 0.0585 (1); I41/amd space group, a = 16.0018(3) Å, c = 14.7186(5) Å, V = 3768.81(16) Å3, d x = 3.169 g/cm3, R = 0.0489 (2); P21/c space group, a = 9.0452(4) Å, b = 15.8065(7) Å, c = 15.2951(6) Å, β = 103.700(2)°, V = 2124.57(16) Å3, d x = 2.957 g/cm3, R = 0.0245 (3). Molecular cluster complexes interact via π-π stacking affording 3D frameworks in 1 and 2 and chains in 3.  相似文献   

20.
Two new isostructural zinc(II) complexes, [ZnCl2(L)] (I) and [ZnBr2(L)] (II), derived from the Schiff base ligand (1-pyridin-2-ylethylidene)pyridin-2-ylmethylamine (L), have been prepared and characterized by physicochemical methods and single-crystal X-ray crystallography. The crystal of I is monoclinic: space group P21/c, a = 11.699(3) Å, b = 8.460(2) Å, c = 14.766(3) Å, β = 99.686(3)°, V = 1440.6(6) Å3, Z = 4. The crystal of II is monoclinic: space group P21/n, a = 8.166(2) Å, b = 15.153(3) Å, c = 11.966(2) Å, β = 96.964(2)°, V = 1469.7(5) Å3, Z = 4. The geometry of the pentacoordinated zinc atoms in both complexes is best described as a square pyramid.  相似文献   

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