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1.
Thomas C. W. Mak 《Journal of inclusion phenomena and macrocyclic chemistry》1990,8(1-2):199-214
The title complexes (1, X = F;2, X = C 1; 3, X = Br and isomorphous with2; 4, X = I) have been prepared and characterized by X-ray crystallography. Crystal data, MoKα radiation:1, space groupCc,Z =4,a = 12.017(3),b = 14.263(5),c = 17.210(7) Å,β = 103.06(2)°, andR F =0.053 for 2044 observed data;2, space groupCc,Z = 4,a = 12.817(3),b = 11.072(2),c = 16.781(5) Å,β =90.74(2)°,R F = 0.044 for 2249 data;3,a = 12.873(4),b = 11. 119(2),c = 16.957(2) Å,β = 89.11(2)°,R F = 0.049 for 2059 data;4, space groupP21/n,Z = 4,a = 8.858(2),b = 14.358(3),c = 15.379(3) Å,β = 93.88(1)°,R F = 0.068 for 3119 data. In all four structures each thiourea molecule interacts with adjacent thiourea molecules via N-H ... S hydrogen bonds to give a ribbon-like arrangement, and also forms a pair of ‘chelating’ N-H ... X hydrogen bonds with a halide ion, resulting in an anionic framework (in1–3) or composite ribbon (in4) as a component in the crystal packing. The measured ranges of N... X distances are: 2.819(5)-2.994(7) Å for1, 3.252(3)-3.291(3)Å for 2, 3.353(6)-3.459(6)Å for3, and 3.564(5)-3.680(5) Å for 4. 相似文献
2.
《Polyhedron》1987,6(6):1439-1443
The title compound was prepared by prolonged reaction of Os2(CH3COO)4Cl2 with Hfhp (Hfhp = 6-fluoro-2-hydroxypyridine) in refluxing toluene in the presence of LiCl. The product, Os2(fhp)4Cl (1), is a result of ligand displacement with a concomitant core reduction of Os26+ to Os25+. Crystals were grown by slow diffusion of hexane into a dichloromethane solution of 1. Crystallographic data are as follows: tetragonal crystal system, space group I4mm (No. 107), a = b = 11.000(3) Å, c = 13.142(2) Å, V= 1590(1) Å3, Z = 2. The molecule possesses crystallographic 4mm symmetry, with the OsOs bonds lying along the four-fold axes. The four fhp ligands are arranged in a polar fashion around the diosmium core, blocking one axial site. The second axial position is occupied by a chloride ion. The principal distances in 1 are: Os(1)Os(2) = 2.341(1) Å, Os(1)N = 2.027(12) Å, Os(2)O = 2.014(5) Å, Os(2)Cl = 2.487(7) Å. The title compound was also investigated by several physical methods. The electrochemistry as determined by cyclic voltammetry revealed two processes: a reversible, one-electron reduction at Eox = −0.63 V in dichloromethane and an irreversible oxidation at Eox = +0.95 V in dichloromethane vs Ag-AgCl at room temperature. The electronic spectrum shows strong bands at 413 nm (ε = 4290 M−1 cm−1), 309 nm (ε = 23,560 M−1 cm−1) and at 294 nm (ε = 26,500 M−1 cm−1) as well as shoulders at 334 and 261 nm. 相似文献
3.
Single-crystal X-ray diffraction is used to determine the structure of a new compound based on an octahedral cyanide anionic cluster complex of rhenium and a trimethyltin(IV) cation: {(SnMe3)3[Re6Se8(CN)6]} (1). The crystallographic characteristics: space group C2/c, a = 13.9898(14) Å, b =15.334(2) Å, c = 20.761(2) Å, β = 97.75(0)°, V = 4412.91(90) Å3, Z = 4, d x = 3.607 g/cm3, and R = 0.0526. The compound has a framework structure; two porous frameworks with pcu topology interpenetrate each other. 相似文献
4.
《Polyhedron》1987,6(7):1577-1585
Reaction of [ReOCl3(PPh3)2] with bromophenylhydrazine in methanol yields [ReCl(N2C6H4Br)2(PPh3)2] (1). Complex 1 reacts with arylthiolates to give mixtures of [Re(SAr)(N2C6H4Br)2(PPh3)2] (2) and [Re2(SAr)7(NNR)2]−. Complexes 1 and 2 display trigonal bipyramidal geometries with the phosphine ligands occupying the axial sites. A significant feature of the structures is the nonequivalence of the rhenium-diazenido moieties, such that for 1 the ReN(1) and N(1)N(2) distances are 1.80(2) and 1.24(3) Å, while ReN(3) and N(3)N(4) are 1.73(2) and 1.32(3) Å, and for 2 the ReN distances are 1.73(1) and 1.80(2)° with corresponding NN distances of 1.32(2) and 1.25(2) Å. Reaction of (PPh4)[ReO(SPh)4] (3) with unsymmetrically disubstituted hydrazines affords complexes of the type [ReO(SPh)3(NMRR′)] (R = Me, R′ = Ph for 4). Complexes 3 and 4 display distorted square pyramidal geometries with the oxo groups apical. The significant feature of the structure of 4 is the nonlinear ReN(1)N(2) linkage, exhibiting an angle of 145.6(10)°. The angle does not appear to correlate with a significant contribution from a valence form with sp2 hybridization at the α-nitrogen. Crystal data: 1: monoclinic space group, P21/n, a = 12.216(2) Å, b = 19.098(2) Å, c = 20.257(4) Å, β = 106.20(1)°, V = 4538.3(8) Å3 to give Z = 4; structure solution and refinement based on 1905 reflections converged at R = 0.070. 2: monoclinic space group P21/n, a = 14.393(2) Å, b = 18.842(3) Å, c = 20.717(4)Å, β = 110.26(1)°, V = 5270.5(8) Å3 to give Z = 4 for D = 1.53 g cm−1; structure solution and refinement based on 4249 reflections to give R = 0.070. 3: monoclinic space group P21/n, a = 12.531(2) Å, b = 24.577(4) Å, c = 16.922(3) Å, β = 99.06(1)°, V = 5146.2(9) Å3, D = 1.36 g cm−3 for Z = 4, 2912 reflections, R = 0.050. 4: monoclinic space group p21/n, a = 16.137(2) Å, b = 9.863(2) Å, c = 16.668(2) Å, β = 111.12(1)°, V = 2474.7(6) Å3, D = 1.74 g cm−3 for Z = 4, 2940 reflections, R = 0.066. 相似文献
5.
A. Yu. Ledneva S. B. Artemkina P. A. Stabnikov L. V. Yanshole V. E. Fedorov 《Journal of Structural Chemistry》2017,58(4):758-762
A new Mo2O3(dpm)4 compound (I) is synthesized by the interaction of Mo(CO)6 with 2,2,6,6-tetramethylheptanedione-3,5 (dpm). The structure of complex I determined by the XRD method is as follows: triclinic crystal system, space group P–1, a = 10.1780(7) Å, b = 10.1817(6) Å, c = 13.3255(9) Å, α = 110.562(2)°, β = 102.233(2)°, γ = 93.9041(19)°, V = 1248.17(14) Å3. The compound is characterized by IR spectroscopy, mass-spectrometry and thermogravimetric analysis (TGA). 相似文献
6.
Two compounds of the formulae (dppeH2)3[MOCl6]2 ·12H2O I and (dppeH2)3[Mo2Cl9]2II are described. For compound I, which proved to be active in olefin epoxidation, the crystal structure was determined. The rose-pink crystals are triclinic, space group P with a = 13.715(9), b3 = 14.686(7), c = 12.512(7) Å, α = 109.56(4), β = 97,98(4) and γ = 91.27(5)°, V = 2345 Å, Dm = 1.42 and Dc = 1.44 gcm?3, Z = 1. Block-diagonal least squares refinement of the structure has led to a final value of the conventional R factor of 0.049 for the 3914 independent reflections with I > 3σ(I). Bond distances are in the range: MoCl 2.439(2)–2.469(2) Å, and PC 1.771(9)–1.806(8) Å. 相似文献
7.
X-Ray Structure of [{LiOC6H2-2,4,6-(CH3)3}4(THF)3] The title compound crystallized from a THF/OEt2 solution. Its crystal structure (monoclinic, P21/c, a = 21.362(3), b = 13.441(2), c = 17.188(2) Å, β = 98.39(1)°, Z = 4, R = 0,0911, wR2 = 0,2562) is built up by cuban-like tetrameric units. Three of the four Li cations attain a coordination number of four by binding to an additional THF molecule. Li(4) without THF coordination has a short distance to one ortho-methyl group (Li(4)…C(27) 2.669(10) Å). The Li–Oph bonding distances vary from 1.869(10) to 2.051(10) Å (average 1.97 Å); the average bonding distance for Li–OTHF is 2.012(10) Å. Averaged bonding angles for Li–Oph–Li′ and Oph–Li–O′ph amount to 84.4(4)° and 95.4(4)°, respectively. The Li…Li distances significantly differ from each other. They range from 2.556(12) to 2.739(11) Å (average 2.65(1) Å). 相似文献
8.
The 1-(diphenylmethylene)-2-(thiazolo[4,5-b]pyridin-2-yl)hydrazine compound (IV) is synthesized based on a 3-amion-2-chloropyridine precursor and characterized by single crystal X-ray diffraction. The structural analysis reveals that compound IV belongs to the monoclinic system, space group P21/c, a = 11.869(5) Å, b = 13.155(6) Å, c = 10.970(5) Å, β = 102.431(5)°, V = 1672.6(12) Å3, Z = 4. In the crystal structure, the molecular species are linked by intermolecular N-H...N hydrogen bonds into onedimensional chains. 相似文献
9.
《Polyhedron》1999,18(8-9):1135-1140
The preparation of several new gold(I) complexes by chloride metathesis of [AuCl(HL)] [HL=Ph2PNHP(O)Ph2] with either HL or K[Ph2P(E)NP(E)Ph2] (E=S or Se) is described. All compounds were characterised by a combination of 31P{1H}, 1H and IR spectroscopy, microanalysis and X-ray crystallography. X-ray structural studies reveal that [Au(HL)2]Cl [monoclinic, space group P21/c, a=9.0726(3) Å, b=21.0847(6) Å, c=12.0131(3) Å, β=105.1090(10)°, V=2219 Å3, Z=2, final R=3.97] forms a one dimensional polymeric structure in which alternating [Au(HL)2]+ and Cl− ions are linked through intermolecular N–H⋯Cl hydrogen-bonding. In contrast the three-co-ordinate compound [Au{Ph2P(Se)NP(Se)Ph2-Se,Se′}(HL)] [monoclinic, space group P21/a, a=21.6752(5) Å, b=9.1200(10) Å, c=24.0742(7) Å, β=106.080(2)°, V=4573 Å3, Z=4, final R=8.94] forms hydrogen-bonded dimer pairs analogous to that previously observed in non-complexed HL. The X-ray crystal structure of the gold(I) precursor [AuCl(HL)] has also been determined: monoclinic, space group P21/c, a=10.217(8) Å, b=23.256(5) Å, c=20.086(5) Å, β=101.15(4)°, V=4683 Å3, Z=8, final R=5.2. The X-ray crystal structure reveals intermolecular N–H⋯OP hydrogen-bonding between adjacent [AuCl(HL)] molecules forming infinite chains. 相似文献
10.
E. G. Gumbris E. V. Peresypkina A. V. Virovets T. G. Cherkasova 《Russian Journal of Inorganic Chemistry》2012,57(3):337-342
New complexes of composition [Bi(DMSO)8][Fe(NCS)6] (1) and [Al(DMSO)6][Al(NCS)6] (2) have been prepared, and an octahedral hexarodanoaluminate anion has been structurally characterized for the first time. Crystals of compound 1 are triclinic, space group \(P\bar 1\), a = 11.2368(4) Å, b = 11.4063(4) Å, c = 21.0711(9) Å, α = 92.9520(10)°, β = 99.9430(10)°, γ = 111.9290(10)°, V = 2447.69(16) Å3, Z = 2, ρcalc = 1.680 g/cm3, R 1 = 0.0564; crystals of compound 2 are cubic, space group \(Pa\bar 3\), a = 15.8201(4) Å, V = 3959.39(17) Å3, Z = 4, ρcalc = 1.462 g/cm3, R 1 = 0.0475. The bismuth coordination polyhedron BiO8 in compound 1 is a distorted square antiprism with broken square faces (Bi-O, 2.368-2.582 Å). In the structure of 2, the cation disordered in a complex manner has an octahedral configuration (Al-O, 1.888(11)-1.912(11) Å). 相似文献
11.
Two dinuclear complexes [Zn(μ-L)(NO3)(H2O)]2 (1) and [Cu2(μ-L)2(HL)2](NO3)2(C12H8Br2)0.5·H2O (2), (HL = 3-(2-pyridyl)pyrazole, C12H8Br2 = 4,4′-dibromobiphenyl) are synthesized under hydrothermal conditions and characterized by elemental analysis and X-ray single crystal diffraction. Crystal data for 1: triclinic, \(P\bar 1\), a = 8.8478(7) Å, b = 15.0550(11) Å, c = 16.4310(12) Å, α = 107.588(4)°, β = 112.498(3)°, γ = 115.595(3)°, V = 2099.8(9) Å3, Z = 2; for 2: triclinic, \(P\bar 1\), a = 7.2870(15) Å, b = 8.6840(17) Å, c = 9.3290(19) Å, α = 107.588(4)°, β = 112.498(3)°, γ = 115.595(3)°, V = 528.77(18) Å3, Z = 1. Complex 1 and 2 are both dinuclear structures which are further packed into a 1D supramolecular chain and a 3D supramolecular framework via weak C–H…O hydrogen bond interactions respectively. 相似文献
12.
T. V. Koksharova G. G. Sadikov A. S. Antsyshkina I. S. Gritsenko V. S. Sergienko O. A. Egorova 《Russian Journal of Inorganic Chemistry》2006,51(6):895-900
A coordination compound of nickel(II) benzoate with nicotinamide [Ni(C6H5COO)2(L)2(H2O)2] (I) (L is nicotinic acid amide) is synthesized and studied by IR spectroscopy. Its crystal structure is solved by X-ray crystallography. The crystals of compound I are monoclinic: a = 7.152 Å, b = 18.266 Å, c = 10.341 Å, β = 109.24°, V = 1275.4 Å3, Z = 2, space group P21/c. Structural units of a crystal of I are centrosymmetric octahedral complex molecules. The coordination environment of the Ni atom contains two O atoms (Ni-O(1) 2.066(2) Å) and two N atoms (Ni-N(1) 2.091(2) Å) of the monodentate-coordinated benzoate anions and nicotinamide molecules, respectively, as well as two O atoms of the H2O molecules (Ni-O(1w) 2.110(2) Å). 相似文献
13.
P. A. Stabnikov S. I. Dorovskikh N. V. Pervukhina L. G. Bulusheva G. V. Romanenko 《Journal of Structural Chemistry》2014,55(3):488-492
Two bis-chelates M(tmih)2 (M = Cu(II), Ni(II), tmih = (CH3)3C(NCH3)CHCOC(CH3)3)? are synthesized and their crystal structures are determined using XRD (Bruker APEX-II diffractometer with a CCD detector, λMoK α, λCuK α, graphite monochromator, T = 240(2) K and 296(2) K): Cu(tmih)2 (I) (space group P21/c, a = 12.9670(8) Å, b = 18.4921(9) Å, c = 11.0422(6) Å, β = 93.408(4)°, V = 2643.1(3) Å3, Z = 4) and Ni(tmih)2 (II) (space group P21/c, a = 12.810(2) Å, b = 18.529(2) Å, c = 11.243(2) Å, β = 91.959(7)°, V = 2667.1(6) Å3, Z = 4). The complexes are isostructural; the coordination polyhedron of metal atoms is a flattened tetrahedron formed from two O atoms (Cu-O of 1.901(2) Å, 1.892(2) Å, Ni-O of 1.845(2) Å, 1.833(2) Å) and two N atoms (Cu-N of 1.976(3) Å, 1.972(3) Å, Ni-N of 1.911(2) Å, 1.920(2) Å) of the ligand; the chelate OMN angles (M = Cu(II), Ni(II)) are in the 87.4–93.1° range; the OMO and NMN angles are 162.2° and 167.2° in I, 171.1° and 173.2° in II. The complexes have the molecular structures formed from isolated molecules bonded by van der Waals interactions. Using a quantum chemical hybrid M06 method, the structures of copper(II) chelates with the H, CH3, CH2CH3, CH(CH3)2, and C(CH3)3 substituents at the nitrogen atom are calculated. Found that with a bulky substituent at the nitrogen atom, the formation of chelates is hindered due to the intraligand repulsion between the atoms of this substituent and the tert-butyl group. 相似文献
14.
Nazan Ocak İskeleli Hasan Karabıyık Çiğdem Albayrak Hande Petek Erbil Ağar 《Structural chemistry》2006,17(4):393-399
The crystal and molecular structure of 2-methyl-4-(4-methoxyphenylazo)phenol have been determined by X-ray single crystal diffraction technique. The compound crystallizes in the monoclinic space group P21/c with a=9.7763(8) Å, b=11.3966(8) Å, c=11.9531(8) Å and β=108.752(6)°. In addition to the molecular geometry from X-ray experiment, its optimized molecular structure has been obtained with the aid of PM3 semiempirical quantum mechanical method, and then the corresponding geometric parameters were compared with those of X-ray crystallography. To determine conformational flexibility and crystal packing effects on the molecules, molecular energy profile of the title compound was obtained with respect to two selected degrees of torsional freedom, which were varied from ?180° to +180° in steps of 10°. Crystal structure of the title compound is a fibroid structure constructed by C–H···O and O–H···N type intermolecular hydrogen bonds. The most favorable conformer of the title compound has been determined by the crystal packing effects and there is no steric hindrance during rotation around the selected torsion angles. 相似文献
15.
Reactions of E-4-ferrocenylpent-3-en-2-one with S-methyldithiocarbazate or S-benzyldithiocarbazate result in the formation of methyl 5-ferrocenyl-3,5-dimethyl-2-pyrazoline-1-dithiocarboxylate (1) or benzyl 5-ferrocenyl-3,5-dimethyl-2-pyrazoline-1-dithiocarboxylate (2). The single crystals of both products are obtained and their structures are identified by X-ray diffraction method with triclinic P-1 space groups. The cell parameters for compound 1 are as follows: a = 7.7029(8) Å, b = 10.1631(11) Å, c = 10.7305(12) Å, α = 101.3270(10)°, β = 90.6740(10)°, γ = 94.8390(10)°, and V = 820.40(15) Å3. For compound 2, the crystallographic data are: a = 7.953(3) Å, b = 10.970(5) Å, c = 12.534(3) Å, α = 84.718(5)°, β = 81.651(3)°, γ = 76.274(4)Å, and V = 1049.1(7) Å3. 相似文献
16.
T.-T. Xu X.-Y. Xu J. Gao Sh.-Sh. Ni D.-Q. Wang L.-D. Lu X.-J. Yang X. Wang 《Journal of Structural Chemistry》2007,48(1):193-197
Two new Schiff bases were prepared by the condensation reaction of paeonol with ethylenediamine (for compound 1) and 1,3-propylenediamine (for compound 2). The compounds were studied with single crystal X-ray diffraction method. Compound 1 is monoclinic, space group P21/c, a = 10.956(15) Å, b = 6.767(10) Å, c = 12.494(18) Å; β = 104.66(2)°, V = 896(2) Å3, Z = 2. Compound 2 is triclinic, space group P-1, a = 6.878(2) Å, b = 12.141(4) Å, c = 12.414(4) Å; α = 101.023(6)°, β = 103.415(6)°, γ = 102.337(6)°, V = 952.8(6) Å3, Z = 2. The molecular structures of 1 and 2 are similar; the molecule being centrosymmetric in 1 but asymmetric in 2. 相似文献
17.
H. -Q. Ye Y. -Y. Li R. -K. Huang X. -P. Liu W. -Q. Chen J. -R. Zhou L. -M. Yang C. -L. Ni 《Journal of Structural Chemistry》2014,55(4):691-696
A new ion-paired compound [4NO2BzPy]2[Co(NCS)4] (1) ([4NO2BzPy]+ = 1-(4′-nitrobenzyl)pyridinium, NCS? = isothiocyanate) is synthesized and characterized by elemental analysis, IR and UV-Vis spectra, ESI-MS and single crystal X-ray diffraction. Compound 1 is orthorhombic, space group Pbcn, with a = 13.188(2) Å, b = 8.458(1) Å, c = 29.281(4) Å, V = 3266.2(7) Å3, D calc = 1.468 g/cm3, Z = 4, F(000) = 1476, R 1 = 0.0332. The [Co(NCS)4]2? anions form an unusual layer structure by S…N and S…Co interactions, while the [4NO2BzPy]+ cations stack into a 1D column by the p…π stacking interaction in the solid state of 1. A magnetic measurement in the range 2–300 K shows a weak antiferromagnetic exchange with θ = ?2.42 K in 1. 相似文献
18.
Two manganese coordination polymers, [Mn2(ip)2(dmf)]·dmf (1) and [Mn4(ip)4(dmf)6]·2dmf (2) (ip=isophthalate; dmf=N,N-dimethylformamide), have been synthesized and characterized. X-ray crystal structural data reveal that compound 1 crystallizes in triclinic space group P?1, a=9.716(3) Å, b=12.193(3) Å, c=12.576(3) Å, α=62.19(2)°, β=66.423(17)°, γ=72.72(2)°, Z=2, while compound 2 crystallizes in monoclinic space group Cc, a=19.80(3) Å, b=20.20(2) Å, c=18.01(3) Å, β=108.40(4)°, Z=4. Variable-temperature magnetic susceptibilities of compounds 1 and 2 exhibit overall weak antiferromagnetic coupling between the adjacent Mn(II) ions. 相似文献
19.
Yu. V. Kokunov V. V. Kovalev G. A. Razgonyaeva Yu. E. Gorbunova S. A. Kozyukhin 《Russian Journal of Coordination Chemistry》2014,40(6):366-370
The reactions of CdI2 with dimethylpyridines (Me2Py is C7H9N) afford complexes CdI2(2,3-Me2Py)2] (I), [CdI2(2,6-Me2Py) (II), and CdI2(3,5-Me2Py)2 (III). The structures of compounds I and II are determined. The crystals of complex I are orthorhombic, space group Pbca, a = 7.930(1) Å, b = 15.537(1) Å, c = 29.943(1) Å, V = 3689.1(5) Å3, ρcalcd = 2.090 g/cm3, Z = 8. The crystals of complex II are monoclinic, space group C2/c, a = 14.784(1), b = 11.991(1), c = 17.711(1) Å, β = 90.39(1)°, V = 1081.1(2) Å3, ρcalcd = 2.908 g/cm3, Z = 4. The structure of compound I is built of discrete neutral complexes [CdI2(2,3-Me2Py)2]. The Cd polyhedron is a distorted tetrahedron (Cd-I 2.289–2.295, Cd-N 2.708–2.734 Å, angles N(I)CdN(I) 103.1°-114.8°). Polymer chains [CdI2(2,6-Me2Py)]∞ extended along the direction [100] are observed due to the bridging iodine atoms in structure II. The Cd polyhedron is a trigonal bipyramid containing iodine atoms at the axial vertices (Cd-Iaks 3.040 Å) and two iodine atoms and the nitrogen atom of the Me2Py ligand in the equatorial plane Me2Py (Cd-Ieq 2.840 Å, Cd-N 2.309 Å). The compounds in the solid state are photoluminescent. 相似文献
20.
B. V. Bukvetskii A. G. Mirochnik P. A. Zhikhareva V. E. Karasev 《Journal of Structural Chemistry》2006,47(3):575-580
The crystal structure of [Eu(TTA)2(NO3)(TPPO)2] (I) (TTA = thenoyltrifluoroacetone, TPPO = triphenylphosphine oxide) possessing intense triboluminescence was established by X-ray crystallography. The crystals are triclinic, noncentrocymmetrical: a = 11.047(3) Å, b = 11.794(3) Å, c = 12.537(3) Å; α = 102.635 (4)°, β = 102.088(4)°,γ = 117.765(3)°; space group P1, Z = 1. The central Eu(III) atom coordinates two oxygen atoms of two TPPO molecules at distances of 2.271 Å and 2.282 Å, two oxygen atoms of the nitrate group at distances of 2.478 Å and 2.481 Å, four oxygen atoms of two TTA ions at distances of 2.365 Å, 2.381 Å, and 2.363 Å, 2.371 Å (coordination number is 8). The coordination polyhedron of the Eu(III) atom is a distorted dodecahedron. Possible reasons for spectral differences in the Stark structure of photo-and triboluminescence of I are discussed. 相似文献