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1.
Crystals of the copper bromide complexes with N-allylisoquinolinium halides of the composition [C9H7N(C3H5)]2CuIICl2.86Br1.14 (I), [C9H7N(C3H5)]CuIBr2 · H2O (II), and [C9H7N(C3H5)]CuIBr2 (III) are prepared by ac electrochemical synthesis, and their structures are studied by X-ray diffraction analysis (DARCh-1 (for I) and KUMA/CCD (for II and III) diffractometers). The crystals of compound I are monoclinic: space group P21/n, a = 15.053(5) Å, b = 10.486(4) Å, c = 17.179(10) Å, γ = 109.77(3)°, V = 2552(4) Å3, Z = 4. The crystals of complex II are triclinic: space group P $\overline 1 $ , a = 7.040(1) Å, b = 7.610(2) Å, c = 12.460(2) Å, α = 79.54(3)°, β = 86.73(3)°, γ = 89.51(1)°, V = 655.4(2) Å3, Z = 2. The crystals of complex III are monoclinic: space group P21/n, a = 12.799(1) Å, b = 7.692(1) Å, c = 13.491(1) Å, β = 111.08(1)°, V = 1239.3(2) Å3, Z = 4. The structure of compound I is built of the CuIIX 4 2? tetrahedra and N-allylisoquinolinium cations united by the C-H···X contacts into corrugated layers. The crystal structure of π-complex II is formed of dimers of the composition [C9H7(C3H5)]2 Cu 2 I Br4 forming layers in the direction of the z axis due to the C-H···X contacts. An important role in structure formation belongs to water molecules that cross-link the organometallic layers through the O-H···X contacts into a three-dimensional framework. When kept in the mother liquor for 6 months, the crystals of compound II transformed into crystals of compound III, whose structure consists of {[C9H7(C3H5)]2Cu 2 I Br4} n columns united through the C-H···Br contacts (H···Br 2.84(3)?2.92(4) Å) into a three-dimensional framework.  相似文献   

2.
Complexes RbL (I) and [Li2(C2H5OH)L2] (II) (L = C23H15O3) have been synthesized and their crystal structures have been studied. Both compounds have monoclinic crystals with space group P21/c and Z = 4; I: a = 11.632(2) Å, b = 15.154(3) Å, c = 11.457(2) Å, β = 104.34(3)°; II: a = 12.982(3)Å, b = 12.083(2) Å, c = 25.317(5) Å β = 100.11(3)°. In the structure of I, dimeric groups [Rb2O6] with a shared edge are linked by the ligands to give infinite layers perpendicular to the x axis and cavities that form oblong channels. In the structure of II, Li2O7 dimers are formed by vertex sharing. The coordination of one of the lithium atoms (Li(1)) is completed to tetrahedral by the oxygen atom of the ethanol molecule. The structure of II, like that of I, is layered.  相似文献   

3.
Reactions of a solution of AgNO3 in aqueous methanol with solutions of 1,4-diallylpiperazine (acidified with HNO3 to pH = 4) and 1-allyloxybenzotriazole in ethanol gave the crystalline silver(I) π-complexes [Ag2(C4H8N2(C3H5)2(H+)2)(H2O)2(NO3)2](NO3)2 (I) and [Ag(C6H4N3(OC3H5)(NO3))] (II). Their crystal structures were determined by X-ray diffraction. Crystals of complexes I and II are monoclinic, space group P21/c; for I: a = 7.053(3)Å, b = 9.389(3)Å, c = 15.488(4)Å, β = 91.60°, V = 1025.3(6)Å3, Z = 4; for II: a = 10.650(4)Å, b = 15.062(5)Å, c = 7.412(4)Å, β = 104.20(3)°, V = 1152.6(8)Å3, Z = 4. In both structures, the organic components act as bidentate ligands forming with AgNO3 34- and 14-membered topological rings, respectively. In complex I, the nearly tetrahedral environment of the Ag(I) atom is made up of the olefinic C=C bond, the O atoms of the nitrate anions, and the water molecule. 1-Allyloxybenzotriazole in structure II causes the deformation of the coordination polyhedron of Ag into a trigonal pyramid via inclusion of the ligand N atom in its coordination sphere. The topological units of the complexes form infinite polymer layers linked by anionic NO 3 ? bridges. In structure I, these layers are united through a system of hydrogen bonds into a three-dimensional framework.  相似文献   

4.
3-Phenylpropenal thiosemicarbazone hydrate C6H5-HC=CH-CH=N-NH-C(S)-NH2 · H2O (HL · H2O, I) and two chelates [Ni(L)2] · nCH3OH (II) and [Zn(L)2] (III) are studied by X-ray diffraction. The crystals of I are orthorhombic: a = 6.227(1) Å, b = 7.763(2) Å, c = 25.585(5) Å, β = 90°, space group P212121, Z = 4, R = 0.0426. A nonplanar molecule of I has an E conformation. The crystals of II are triclinic: a = 6.551(2) Å, b = 10.752(3) Å, c = 10.885(3) Å, α = 64.751(5)°, β = 82.753(5)°, γ = 89.857(5)°, space group, Z = 1, R = 0.0661. In a centrosymmetric molecule of II, the central atom coordinates two deprotonated ligands L through the immine nitrogen atom and thioamide sulfur atom at the vertices of a distorted square. The crystals of III are monoclinic: a = 25.342(2) Å, b = 9.150(2) Å, c = 21.340(3) Å, α = 90°, β = 111.84(2)°, γ = 90°, space group C2/c, Z = 8, R = 0.0556. In a molecule of complex III, two deprotonated bidentate ligands L are coordinated by the zinc ion through the immine nitrogen atoms and thioamide sulfur atoms to form a distorted tetrahedron at the central atom. In both II and III, ligand L after coordination by the metal ion changes the E conformation with respect to the N(1)-C(2) bond for the Z conformation. In crystals I-III, molecules are packed to form infinite layers parallel to the planes (001) and (010).  相似文献   

5.
Two complexes are synthesized: diaquabromo(18-crown-6)rubidium [RbBr(18-crown-6)(H2O)2] (I) and triaqua(18-crown-6)barium dibromide monohydrate [Ba(18-crown-6)(H2O)3]2+ 2Br? · H2O (II). The orthorhombic structure of compound I (space group Pnma, a = 10.124 Å, b = 15.205 Å, c = 12.544 Å, Z = 4) and the monoclinic structure of compound II (space group C 2/c, a = 17.910 Å, b = 10.315 Å, c = 14.879 Å, β = 123.23°, Z = 4) are determined by a direct method and refined by the full-matrix least-squares method in the anisotropic approximation to R = 0.063 (I) and 0.042 (II) for all 2293 (I) and 3363 (II) independent measured reflections (CAD-4 automated diffractometer, λMoK α). The complex molecule [RbBr(18-crown-6)(H2O)2] in compound I and the randomly disordered cation [Ba(18-crown-6)(H2O)3]2+ in compound II are of the host-guest type: their Rb+ or Ba2+ cation (its coordination number is nine) is located in the cavity of the 18-crown-6 ligand and coordinated by all six O atoms. In structure I, the coordination polyhedron of Rb+ is a distorted hexagonal pyramid with a triple apex at the Br? ligand and two O atoms of the water molecules. In structure II, the Ba2+ polyhedron is a distorted hexagonal bipyramid with one apex at the O atom of the water molecule and the other split apex at two O atoms of water molecules.  相似文献   

6.
Two new coordination polymers, [Pb(IDPT)2(NO3)2] (I) and [Mn(IDPT)(SO4)(H2O)2] (II) (IDPT = imidazo[4,5-f][1,10]phenanthroline), were synthesized by hydrothermal method and characterized by elemental analysis and single-crystal X-ray diffraction technique. The results reveal that the complex I belongs to monoclinic crystal system, space group C2/c and complex II belongs to monoclinic crystal system, P21/c space group. The cell parameters are: a = 19.1970(13), b = 7.3875(5), c = 17.3825(12) Å, β = 100.47(10)°, V = 2424.0(3) Å3, Z = 4, F(000) = 1488 for I; a = 10.9135(6), b = 7.0230(4), c = 19.7034(10) Å, β = 99.32(10)°, V = 1490.25(14) Å3, Z = 4, F(000) = 828 for II. In the structure of complex I, the metal center Pb(II) is six-coordinated, displays an octahedral geometry. Each molecule is further connected with neighboring one via π-π interactions into 1D chain. In complex II, Mn(II) is six-coordinated to form a distorted octahedral geometry. Compound II displays 1D supramolecular chain formed through hydrogen bonds. Additionally, the fluorescent properties for the complexes were investigated. Complexes I and II exhibit strong photoluminescence with emission maximum at 583 and 529 nm at room temperature.  相似文献   

7.
Thulium trifluoroacetate compounds have been synthesized, Tm(CF3COO)3 · 3H2O (I) and Tm2(CF3COO)6 · 2CF3COOH · 3H2O (II). The structure of I has been refined by the Rietveld method on the basis of the structural data for Cd(CF3COO)3 · 3H2O. The structure of II has been solved in a single-crystal X-ray diffraction study. Compound I has been studied by thermal analysis. Crystals of I and II are monoclinic: for I a = 9.062(2) Å, b = 18.678(3) Å, c = 9.687(2) Å, β = 113.93(1)°, Z = 2, space group P21/c, R 1 = 0.062; for II a = 8.560(4) Å, b = 19.866(5) Å, c = 20.813(7) Å, β = 101.69(4)°, Z = 8, space group C2/c, R 1 = 0.0392. In the molecular structure of I, thulium atoms are bonded in pairs through four bridging trifluoroacetate anions to form dimers. The coordination polyhedron of the thulium atom also includes the three O atoms of the water molecules and the O atom of the monodentate trifluoroacetate group; the coordination number of the thulium atom is eight. In the chain structure of II, there are two crystallographically independent thulium atoms with coordination numbers 8 and 9. The coordination polyhedra of the Tm(1) and Tm(2) atoms are a distorted monocapped tetragonal antiprism and a distorted tetragonal antiprism, respectively. The Tm-O bond lengths are in the range 2.28(1)–2.85(2) Å. The thulium atoms are bound into chains through carboxylate groups. These chains are linked into layers through hydrogen bonds.  相似文献   

8.
The crystals of copper(I) π-complexes with N-allyl piperazine derivatives, [C3H5NH(CH2)4NH2]Cu2Cl4(I) and [C3H5NH(CH2)4NHC3H5]0.5CuCl2(II), were prepared by alternating-current electrochemical synthesis. X-ray diffraction study showed that compounds Iand IIcrystallize in the monoclinic system: for I, space group P21/a, a= 10.254(4) Å, b= 12.306(4) Å, c= 10.656(4) Å, γ = 98.83(3)°, V= 1329(2) Å3, Z= 4, R= 0.0457 for 1334 independent reflections; for II, space group P21/n, a= 10.187(2) Å, b= 7.283(2) Å, c= 10.480(3) Å, γ = 100.72(2)°, V= 764.0(6) Å3, Z= 4, R= 0.0371 for 1025 independent reflections. The structure of Iis composed of {Cu2Cl4(C7H16N2)}2dimers linked by fairly strong (N)H···Cl hydrogen bonds (2.35(4) Å). The structure of IIconsists of centrosymmetrical dimeric Cu2Cl4 2–anions, whose copper atoms coordinate the allyl groups of different centrosymmetrical organic cations. The dimer–ligand chains are stretched along the [ $ {11} $ 0] direction and are joined by hydrogen contacts (N)H···Cl (2.62(4) Å).  相似文献   

9.
Alternating-current electrochemical synthesis is used to obtain for the first time halogenocuprates of an allyl derivative of phosphonium of the composition (CH2=CHCH2(C6H5)3P)CuX2 (X = Br (I), Cl (II)). Compound I crystallizes in the space group P21, a = 9.6341(3) Å, b = 12.4167(4) Å, c = 9.9618(4) Å, β = 117.484(5)°, Z = 2. Compound II crystallizes in the space group P21/n, a = 9.9725(5) Å, b = 15.4586(8) Å, c = 13.7557(5) Å, β = 90.429(4)°, Z = 4. In the structures of I and II quasilinear CuX 2 ? anions are held by C-H…X hydrogen bonds inside a framework formed by the stacking of phenyl groups from CH2=CHCH2(C6P5)3P+ cations. Allyl groups are not involved in coordination with copper(I) atoms.  相似文献   

10.
New (C17H20FN3O3)2[CoCl4]2·3H2O (I) and C17H20FN3O3[CoCl4]·H2O (II) compounds, where C17H18FN3O3 is ciprofloxacin (CfH), are synthesized and their crystal structures are determined. Crystallographic data for I: a = 18.441(5) Å, b = 9.030(3) Å, c = 27.551(8) Å, V = 4588(4) Å3, space group Pca21, Z = 4; for II: a = 9.305(3) Å, b = 9.885(3) Å, c = 12.999(4) Å, α = 82.782(4)°, β = 72.954(4)°, γ = 89.736(4)°, V = 1133(1) Å3, P-1 space group, Z = 2. Both structures contain CfH 3 2+ ion pairs bonded by the π-π interaction. Additionally, in the crystal of I there is a stacking interaction between the π clouds of aromatic rings and hydrogen atoms of the cyclopropyl group linking the pairs of molecules with each other. The structure of the centrosymmetric crystal of triclinic phase II is also formed from CfH 3 2+ ion pairs bonded by the π-π interaction, which, in this case, are not independent because they are related by the symmetry center. Hydrogen bonds form a branched three-dimensional network linking the CfH 3 2+ and CoCl 4 2? ions and water molecules.  相似文献   

11.
Tetraamminecobalt hydrogen hexamolybdoferrate [Co(NH3)4] · H[FeMo6O18(OH)6] · 6H2O (I) and tetraamminecobalt hydrogen hexamolybdogallate(III) [Co(NH3)4] · H[GaMo6O18(OH)6] · 6H2O (II) were synthesized and studied by mass spectrometry, thermogravimetry, IR spectroscopy, and X-ray diffraction. Crystals of I and II are monoclinic; a = 16.21 Å, b = 5.43 Å, c = 12.32 Å, β = 119.63°, V = 1092.11 Å3, ρcalcd = 2.21 g/cm3, and Z = 1 for I; a = 16.24 Å, b = 5.59 Å, c = 12.29 Å, β = 119.79°, V = 1064.05 Å3, ρcalcd = 2.15 g/cm3, and Z = 1 for II. Compounds I and II were used as catalysts for soft oxidation of natural gas.  相似文献   

12.
It has been shown that N,N’-diaryldiaza-18-crown-6 ethers with p-dimethylamino-and p-methoxy groups in the benzene ring (aryl is 4-Mc2NC6H4) (I) and 4-MeOC6H4 (II) form complexes with potassium and barium salts. The influence of these salts on the UV and 1H NMR spectra of crown ethers I and II has been studied. The stability constants (logβ) of the complexes increase in the series II · Ba(ClO4)2 (2.0), I · Ba(ClO4)2 (2.3), II · KBr (2.8), I · KBr (3.0). N,N’-bis(4-dimethylphenylamine)diaza-18-crown-6 (L, I) and its complex with barium perchlorate Ba(ClO4)2 · L (III) are characterized by X-ray crystallography. The crystals of I are monoclinic: a = 13.778(2) Å, b = 5.9731(9) Å, c = 17.542(3) Å, β = 106.65(1)°, V = 1383.1(4) Å3, Z = 2, space group P21/n, R = 0.0374 for 990 reflections with I > 2σ(I). The crystals of III are monoclinic: a = 17.275(4) Å, b = 8.017(2) Å, c = 26.935(4) Å, β = 100.47(2)°, V = 3669(1) Å3, Z = 4, space group C2/c, R = 0.0320 for 1897 reflections with I > 2σ(I). The molecules of I and III are centrosymmetric. In III, the Ba atom is in the center of substituted diaza-18-crown-6 (DA18C6). The Ba atom is coordinated by all six donor atoms of diaza-18-crown-6 (av. Ba-O, 2.779(3) Å; Ba-N, 3.004(4) Å) and four oxygen atoms of two asymmetrically bound perchlorate groups (Ba-O, 2.832(4) and 3.031(4) Å) arranged below and above the plane of substituted diaza-18-crown-6. The conformations of the macrocycle in free and coordinated L are different.  相似文献   

13.
The reaction of K2[Ru(NO)Cl5] with pyridine in aqueous ethanol at pH ~ 7–8 affords a nitrosoruthenium hydroxocomplex mer-[Ru(NO)Py3Cl(OH)]Cl·1.5H2O (I) (yield ~55%). Treatment of hydroxocomplex I with hydrochloric acid at room temperature gives the aqua complex mer-[Ru(NO)Py3Cl(H2O)]Cl2·2H2O·0.5HCl (II). The structures of the compounds are determined by X-ray crystallography: I, space group P21/n, a = 9.2292(4) Å, b = 11.7781(4) Å, c = 17.4915(7) Å, β = 90.9560(10)°, R = 4.84%; II, space group P-1, a = 7.3528(9) Å, b = 11.5793(11) Å, c = 13.6961(16) Å, α = 84.558(3)°, β = 87.668(4)°, γ = 74.146(4)°, R = 6.22%. Compounds I and II are characterized by powder XRD, 1H and 13C NMR, and IR spectroscopy. The thermal decomposition of compound II in the inert atmosphere is examined by thermal analysis.  相似文献   

14.
Cs2[(UO2)2(C2O4)3] (I) and Cs2[UO2(C3H2O4)2] · H2O (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) Å3, space group P21/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) Å3, space group P21/c, Z = 4, and R 1 = 0.0287 for II. The uranium-containing structural units of complexes I and II are [(UO2)2(C2O4)3]2? chains and [UO2(C3H2O4)2] 2 4? dimers, which belong to the AK 0.5 02 T11 and AT11B01 crystallochemical groups (A = UO 2 2+ , K02 and T11 = C2O 4 2? , T11 and B01 = C3H2O 4 2? ) of uranyl complexes.  相似文献   

15.
Solvate Ph3Sb[OC(O)C6H4(OH-4)]2 · 1/2Et2O (I) has been synthesized by the reaction between triphenylantimony and 4-oxybenzoic acid in the presence of hydrogen peroxide in diethyl ether. Tetraphenylantimony 4-oxybenzoate, which crystallizes from DMSO in the form of solvate Ph4SbOC(O)C6H4(OH-4) · DMSO (II), has been synthesized from pentaphenylantimony and triphenylantimony bis(4-oxybenzoate) or 4-oxybenzoic acid. According to X-ray diffraction data, an antimony atom in molecules of compounds I and II has a trigonal bipyramidal coordination. Crystals of compound I contain two crystallographically independent types of molecules (A and B). The Sb-C and Sb-O distances, the equatorial CSbC and axial OSbO angles are, respectively, 2.083(9)–2.103(8)Å; 2.068(5), 2.128(5)Å; 117.6(3)°–124.2(3)° and 171.5(2)° (IA); 2.103(9)–2.135(8)Å; 2.086(5), 2.154(6)Å;110.2(3)°–138.0(4)° and 174.8(2)° (IB). In compound II, Sb-C is 2.117(2)–2.175(2) Å, Sb-O is 2.247(2) Å, and CeqSbCeq and OSbCax angles are 110.89(9)°–133.30(9)° and 177.05(7)°, respectively. The Sb…O=C intramolecular contacts are 3.151(7), 3.153(8) Å (IA), 2.985(8), 3.008(9) Å (IB), and 2.975(5) Å (II). Molecules IA and IB are conformation isomers, which differ from each other by the arrangement of carboxyl groups with respect to the equatorial plane.  相似文献   

16.
Interaction of salts of the cluster anions {Re [Re6Q8(CN)6]4?/3? (Q = Se, Te) with Nd salts in the presence of 2,2′-bipyridyl (Bipy) ligand brings about new coordination polymers: Pr 4 n N[{Nd(Bipy)(H2O)4} {Re6Se8(CN)6}] · 2H2O (I) (space group C2/c, a = 18.2918(16) Å, b = 14.9972(13) Å, c = 37.513(3) Å, β = 102.046(4)°, V = 10064.2(15) Å3, Z = 8), [{Nd(Bipy)2(H2O)} {Re6Se8(CN)6}] (II) (space group C2/c, a = 15.8668(3) Å, b = 13.5403(3) Å, c = 20.5189(4) Å, β = 110.135(1)°, V = 4138.89(15) Å3, Z = 4), and [{Nd(Bipy)(EtOH)(H2O)4}{Re6Te8(CN)6}] · EtOH (III) (space group $P\bar 1$ , a = 9.4733(6) Å, b = 12.5326(8) Å, c = 17.2374(11) Å, α = 96.561(2)°, β = 90.310(2)°, γ = 94.876(2)°, V = 4138.89(15) Å3, Z = 4). The compounds synthesized are characterized by single-crystal X-ray diffraction and IR methods. Compounds I and III have layered (2D) structures, compound II is a framework (3D) polymer.  相似文献   

17.
Four new fluorochromatouranylates, namely, K[UO2(CrO4)F] · 1.5H2O (I), Rb[UO2(CrO4)F] · 1.5H2O (II), Rb[UO2(CrO4)F] · 0.5H2O (III), and Cs[UO2(CrO4)F] · 0.5H2O (IV), have been synthesized, and their crystallographic characteristics have been determined. All the compounds crystallize in monoclinic system, space group P21/c, with the unit cell parameters a = 13.1744(5) Å, b = 9.4598(3) Å, c = 13.0710(4) Å, β = 103.746(1)°, Z = 4, R = 0.0235 (I); a = 13.5902(7) Å, b = 9.5022(4) Å, c = 13.2271(6) Å, β = 102.914(2)°, Z = 4, R = 0.0247 (II); a = 24.7724(8) Å, b = 12.6671(4) Å, c = 9.4464(3) Å, β = 97.661(1)°, Z = 8, R = 0.0448 (III); a = 25.725(1) Å, b = 12.8261(5) Å, c = 9.4929(4) β = 97.208(1)°, Z = 8 (IV). The pairs of compounds I and II and compounds III and IV are isostructural. Crystals of compounds I–III have been subjected to complete X-ray diffraction study. It has been established that the structures of compounds I–III are built of [UO2(CrO4)F] n n? layers, which are parallel to the (100) plane and linked into a framework by alkali-metal cations located between layers, together with water molecules. The effect of topological and geometric isomerism on the structural features of 34 known uranyl compounds of the AT3M2 crystallochemical group, to which the studied compounds I–III also belong, is discussed.  相似文献   

18.
[[UO2(L)(OH)] (I), (CN3H6)2[(UO2)2CrO4(L)4] · 2H2O (II), and [UO2(H2O)5][(UO2)2Cr2O7(L)4] (III) crystals, where L is picolinate ion C5H4NCOO?, have been synthesized and studied by X-ray diffraction and IR spectroscopy. Complex I crystallizes in triclinic system with the unit cell parameters a = 6.2858(5) Å, b = 7.9522(5) Å, c = 8.3598(6) Å, α = 79.527(6)°, β = 87.760(6)°, γ = 79.126(6)°, space group P $\bar 1$ , Z = 2, R = 0.0306, and complexes II and III crystalize in monoclinic system with a = 8.8630(9) Å, b = 13.4540(13) Å, c = 31.266(3) Å, β = 93.118(3)°, space group C2/c, Z = 4, R = 0.0187 (II), and a = 7.3172(4) Å, b = 15.4719(8) Å, c = 16.6534(10) Å, β = 98.943(4)°, space group P21/m, Z = 2, R = 0.0588 (III). The structure of complex I is built of electronegative [UO2(L)(OH)] chains, which belong to the AT11M2 crystallochemical group (A = UO 2 2+ , T11 = L, M2 = OH?) of uranyl complexes. The structure of complexes II and III contains [(UO2)2(L′)(L)4]2? dimers (L′ = CrO 4 2? or Cr2O 7 2? ), which belong to the A2B2B 4 01 group (A = UO 2 2+ ,B2 = L′, B01 = L). The specifics of intermolecular interactions in the structures of complexes I–III and some their analogues have been considered using molecular Voronoi-Dirichlet polyhedra.  相似文献   

19.
New heteroligand Cu(II) and Zn(II) complexes with the α-naphthylacetic acid anion (NAA) and monoethanolamine (MEA), [M(NAA)2(MEA)2] (M = Cu2+, (I), Zn2+ (II)), are synthesized. The crystal structures of the obtained complexes are determined by X-ray diffraction analysis (CIF files CCDC 984097 (I) and 930946 (II)). The crystals are monoclinic, for I: a = 18.8140(9) Å, b = 4.82500(14) Å, c = 16.0360(7) Å, β = 115.135(6)°, V = 1317.87(11) Å3, space group P21/c, Z = 2; for II: a = 32.9760(14) Å, b = 5.0911(3) Å, c = 15.7994(10) Å, β = 94.418(5)°, V = 2644.6(3) Å3, space group C2/c, Z = 4. In the structure of complex I, the Cu2+ ion arranged in the symmetry center is coordinated at the vertices of the distorted octahedron by the oxygen atoms of two NAA molecules (Cu-O(2) 2.019(4) Å) and two MEA molecules. The latter is the bidentate-chelating ligand and coordinates the metal through the O and N atoms to form the five-membered metallocycle (Cu-O(3) 2.457(5), Cu-N(1) 1.986(5) Å). In complex II, the Zn atom (on axis 2) is coordinated at the vertices of the distorted tetrahedron by the oxygen atoms of two NAA molecules (Zn-O(2) 1.976(4) Å) and the nitrogen atoms of two MEA molecules (Zn-N 2.034(6) Å). The character of the interaction of coordinated NAA and MEA ligands and methods for packing complexes I and II are considered on the basis of the structural data.  相似文献   

20.
Heating of an aqueous solution of [Pt(en)Py2Cl2]Cl2 · 2H2O (I) with KBr excess leads to the formation of [Pt(en)Py2Br2]Br2 · H2O (II). The interaction of a solution of II with bromine water results in the precipitation of polybromide ([Pt(en)Py2Br2]Br2 · Br2), which within a few days in the reaction solution partly transforms into oximide platinum(IV) complex, [Pt(HN-C(O)-C(O)-NH)Py2Br2] · H2O (III). Complex [Pt(en)PyBr3]Br · H2O (IV) with an impurity of II was prepared by reacting KBr excess and the product of [Pt(en)Py2]Cl2 oxidation with chlorine in 0.05 N HCl. The action of HNO3 on the solution of IV produced a nitrate derivative ([Pt(en)PyBr3]NO3, V). Complex IV, unlike II, does not react with bromine. The IR spectra of all the obtained compounds were recorded. Complexes II, III, and V were studied by X-ray crystallography. The crystals of II are monoclinic, space group P21/c, a = 15.640(2) Å, b = 9.345(1) Å, c = 14.167(2) Å, β = 102.63(1)°, V = 2020.5(5) Å3, Z = 4, R hkl = 0.033. The crystals of III are triclinic, space group P $\bar 1$ , a = 7.108(1) Å, b = 10.946(1) Å, c = 11.020(2) Å, α = 83.63(1)°, β = 80.31(1)°, γ = 75.02(1)°, V = 814.4(2) Å3, Z = 2, R hkl = 0.033. In the near-planar five-membered chelate ring (torsion angle NCCN is 7°), the C-O distances (1.23(1) Å) correspond to double bonds; the C-C (1.53(1) Å) and C-N (1.31(1) Å), distances correspond to ordinary bonds. The crystals of V are monoclinic, space group P21/c, a = 8.306(2) Å, b = 8.995(2) Å, c = 20.231(4) Å, β = 97.48(2)°, V = 1498.6(6) Å3, Z = 4, R hkl = 0.037.  相似文献   

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