共查询到20条相似文献,搜索用时 15 毫秒
1.
((CH 3) 2Au) 2C 2O 4 ( 1), ((CH 3) 2AuSCN) 2 ( 2), (CH 3) 2AuSSP(OCH 3) 2 ( 3), and (CH 3) 2AuSSP(OC 2H 5) 2 ( 4) were prepared and recrystallized from hexane to determine their crystal structures and analyze them by thermal methods (TGA). The compounds have been investigated as new possible precursors for metal–organic chemical vapor deposition (MOCVD). Compounds 1 and 2 are solids, while 3 and 4 are liquids. Crystal structures of 1 and 2 have been studied by single-crystal X-ray diffraction (XRD): compounds are monoclinic, space group for 1 P2 1/ c, for 2 P2 1/ n. Compound 1 has crystal parameters a?=?7.6952(5)?Å, b?=?11.1814(8)?Å, c?=?12.2893(8)?Å, α?=?90°, β?=?104.922(4)°, γ?=?90°; 2 has crystal parameters a?=?5.6184(3)?Å, b?=?15.2744(6)?Å, c?=?6.9202(3)?Å, α?=?90°, β?=?102.864(2)°, γ?=?90°. These are neutral complexes, in which molecules are only connected by van der Waal's interactions. Thermal gravimetric analyses (TGA) have shown that 3 and 4 evaporate practically without decomposition. MOCVD experiments were carried out at lower pressure using 3 and 4 as precursors. The films were grown on Si substrate and investigated by XRD and SEM. 相似文献
2.
Crystal growth and characterization by X-ray diffraction and NMR spectroscopy of a new p-phenylenediamonium diphosphate [p-NH 3 C 6 H 4 NH 3] H 2 P 2 O 7 are reported. This compound crystallizes in a triclinic unit cell P1 with the parameters a = 7.130(3), b = 9.047(3), c = 9.350(2) Å, α = 133.44(2)°, β = 95.02(2)°, γ = 107.11(4)°, Z = 2, V = 514.3(15) Å 3, and D x = 1.848 g.cm ? 3. The crystal structure has been solved and refined to R = 0.0273, using 3678 independent reflections. The atomic arrangement is build up by infinite ribbons of [H 2 P 2 O 7] 2? anions, extending along the a-direction at y = 1/2. Between these ribbons are located the p-phenylenediammonium entities, which form hydrogen bonds N─H…O with some external oxygen atoms of phosphoric groups. Crystallographic results are correlated with that of the solid state 13C and 31P MAS NMR spectroscopy. 相似文献
3.
A three-dimensional (3D) supramolecular compound, [(phen)LSnS] 2·(H 2O) 2 (phen = 1,10-phenanthroline, L = mercaptoacetic acid), has been synthesized and the crystal structure was determined by a single crystal X-ray diffraction study. 1 is triclinic, space group P-1 with a = 6.695(1) Å, b = 10.929(2) Å, c = 12.117(2) Å, α = 114.55(3)°, β = 93.53(2)°, γ = 104.06(3)°, and Z = 1. The dinuclear cluster of [(phen)LSnS] 2 and H 2O are linked into a 3D supramolecular framework by a combination of O[sbnd]H…O, C[sbnd]H…O hydrogen bonds and π–π stacking interactions. Its luminescence property is discussed. 相似文献
4.
Abstract The heterometallic polymeric cluster Na 2[AlW 3O 4 (O 2CEt) 8] 2 ( 1) has been prepared by reaction of W(CO) 6 and NaWO 4·2H 2O with AlCl 3 at 120°C in propionic anhydride and characterized by X-ray crystallography, with the following crystal data: triclinic, space group P1, a = 12.205(5), b = 13.032(4), c = 13.925(3) Å, α = 90.21(3)°, β = 109.53(5)°, γ = 117.26(6)°, V = 1822.8(1)Å 3, Z = 1, R = 0.038 and Rw = 0.101. The structure consists of two triangular [W 3O 4(O 2CEt) 8] 4? cluster unit, which act as polydenate ligands to link Al 3+ and Na + ions forming a one–dimensional chain structure. IR spectra show characteristic [W 3O 4] 4+ bands at 746–815 cm ?1. Thermal analysis reveals that the complex is air stable up to 250°C. Cluster 1 decomposes in hot aqueous 2 M HCl solution to produce discrete [W 3O 4] 4+ units. 相似文献
5.
The crystal and molecular structure of the title compound, [Ni(phen) 2(CH 3) 2CHOCSS](CH 3) 2CHOCSS has been determined by X-ray diffraction. The brown crystal is triclinic of space group Pi, with parameters a = 11.790(2), b = 12.410(3), c = 12.680(3) Å, α = 92.49(3), β = 96.54(3), γ = 117.43(3)° and Z = 2. The compound contains a six-coordinate cation and an isopropyl xanthate anion (CH 3) 2CHOCSS ?, the central Ni atom is chelated by four nitrogen atoms of two phenanthroline ligands and two sulfur atoms of an isopropyl xanthate ligand. The TG data indicate that it decomposed completely at 734°C. 相似文献
6.
A new cobalt(II) cyanato complex, [Co(NCO) 2(H 2O) 2(hmt)] ( I) where hmt is hexamethylenetetramine, has been synthesized and structurally characterized. The electronic spectra of the solid compound suggest octahedral cobalt and IR spectra revealed monodentate N-cyanato groups and aqua ligands, while hmt is a bridging N, N′-bidentate leading to a 1-D infinite polymeric chain. The structure has been confirmed from single crystal X-ray diffraction. Crystal data for I : Fw 319.20, a = 9.234(2), b = 11.252(2), c = 12.576(3) Å, β = 107.75(3)°, V = 1244.5(4) Å 3, Z = 4, T = 100 K. Crystal system : monoclinic, space group : C2/c. Hydrogen bonds of the type O–H ··· O and O–H ··· N between aqua molecules and O atom of the terminal N-cyanato groups or an N atom of hmt ligands consolidate and extend the structure to a 3-D network. The thermal properties of I are reported. 相似文献
7.
Abstract It has been shown that host compound 1,1,6,6-tetraphenylhexa-2,4-diyne-1,6-diol is able to include polar guests and now we report on its ability to form clathrate compounds with apolar guests. The structures of this host with cyclohexane (1) and the ortho (2), meta (3) and para (4) xylenes have been determined and are discussed. Crystal data: (1) 2C 30H 22O 2C 6H 12, M r = 913.20 g mol ?1, mono-clinic, C2/ c, a = 22.851(6), b = 14.010(2), c = 17.076(6) Å, β = 108.71(3)°, V = 5178(2) Å 3, Z = 4, D c = 1.17g cm ?3, N = 3326, R = 0.092. (2) 2C 30H 22O 21 ½C 8H 10, M r = 1976.5 g mol ?1, triclinic, P 1, a = 13.185(3), b = 15.466(3), c = 16.573(2) Å, α = 96.39(13)°, β = 106.96(15)°, γ = 114.94(18)°, V = 2822(2) Å 3, Z = 2, D c = 1.16 g cm ?3, N = 6152, R = 0.075. (3) 2C 30H 22O 21 ½C 8H 10, M r = 1976.5 g mol ?1, triclinic, P 1, a = 13.267(5), b = 15.453(3), c = 16.654(5) Å, α = 97.12(2)°, β = 107.09(3)°, γ = 114.68(3)°, V = 2843(2) Å 3, Z = 2, D c = 1.15 g cm ?3, N = 6505, R = 0.083. (4) 2C 30H 22O 21 ½C 8H 10, M r = 1976.5 g mol ?1, triclinic, P 1, α = 13.070(2), b = 15.348(3), c = 16.776(3) Å, α = 67.88<2)°, β = 74.27(1)°, γ = 65.29(1)°, V = 2817(1) Å 3, Z = 2, D c = 1.15 g cm ?3, N = 6711, R = 0.050. Thermal analysis studies were also performed in order to examine their stability and the strength with which the guest species are held in the crystal lattice. 相似文献
8.
Abstract The manganese complexes, [Mn(III)(Hvanpa) 2(NCS)] (1) and [Mn(III)(Hvanpa) 2]Cl · H 2O (2), have been prepared and the crystal structure of complex 2 determined using X-ray crystallography. The monomeric complex has a six-coordinate octahedral geometry. The complex crystallizes in the triclinic space group P-1 with a = 11.446(5) Å, b = 12.782(6) Å, c = 9.023(3) Å, α = 93.92(3)°, β = 97.05(3)°, γ = 65.42(2)°, V = 1169.0(9) Å 3 and Z = 2. The Mn-O and Mn-N distances in the equatorial plane are in agreement with those found for other manganese (III) Schiff-base complexes. In the axial direction, the Mn-O distances of 2.256(3) and 2.236(3) Å, respectively, are about 0.4 Å longer than those in the equatorial plane due to Jahn-Teller distortion at the d 4 manganese(III) center. In the crystal, each chloride ion is linked through hydrogen bonding with two hydrogen atoms from the coordinated hydroxyl groups at the apical site. The lattice water molecules also interact with the phenolic oxygen atoms through hydrogen bonding. 相似文献
9.
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
10.
Two zinc complexes of enoxacin were synthesized and their crystal structures were determined. Compound 1, [Zn(H-Eno) · Cl 2] · 3H 2O (H-Eno = Enoxacin), crystallizes in the triclinic system, space group P 1, with lattice parameters a = 8.7731(12), b = 9.4976(14), and c = 13.2033(19) Å, α = 86.319(7)°, β = 71.912(7)°, and γ = 80.604(7)°, V = 1031.6(3) Å 3, Z = 2, D Calcd = 1.631 Mg m ?3; compound 2, [Zn(H-Eno) · (H 2O) 2] · 2NO 3, also crystallizes in the triclinic system, space group P 1, with lattice parameters a = 8.751(2), b = 9.014(2), and c = 12.594(3) Å, α = 92.277(14)°, β = 109.867(12)°, and γ = 111.469(12)°, V = 854.1(3) Å 3, Z = 1, D Calcd = 1.684 Mg m ?3. 相似文献
11.
A manganese(II) coordination polymer [Mn(TMB) 2?·?H 2O] n ( 1) (HTMB?=?3,4,5-trimethoxybenzoic acid) has been synthesized under hydrothermal conditions and characterized by single-crystal X-ray diffraction, elemental analysis, powder X-ray diffraction analysis, spectroscopic (IR, solid state UV-Vis), and thermal methods. The crystal belongs to orthorhombic system, space group P2 12 12 1, with cell parameters a?=?7.3001(8), b?=?11.4146(13), c?=?27.053(3)?Å, α?=?β?=?γ?=?90°, V?=?2254.3(4)?Å 3, Z?=?4. In 1, TMB in two different coordination modes bridges six-coordinate manganese(II) centers forming a 1-D infinite chain coordination framework. The spectral and thermal properties of the complexes have also been studied. 相似文献
12.
The reaction of MX 2 (M = Co(II), Ni(II); X = Cl, Br) with 2-aminopyrimidine in aqueous acid yields compounds [(2-apmH) 2MX 4], (2-apmH) 2[MX 4], or (2-apmH 2) [MX 2(H 2O) 4]X 2 (2-apmH = 2-aminopyrimidinium; 2-apmH 2 = 2-aminopyrimidinium(2+)). All compounds have been characterized by single crystal X-ray diffraction. The compounds [(2-apmH) 2MX 4] with M = Co, X = Cl ( 1); M = Ni, X = Cl ( 3); and M = Ni, X = Br ( 4) are isomorphous and crystallize as nearly square planar MX 4 units with the 2-apmH cations coordinated in the axial sites through the unprotonated ring nitrogen. (2-ApmH) 2[CoBr 4] ( 2) crystallizes as the salt with a nearly tetrahedral CuBr 4 2- anion. (2-ApmH 2)[NiBr 2(H 2O) 4]Br 2 ( 5) forms as a cocrystal of the neutral, six-coordinate nickel complex and (2-ampH 2)Br 2, stabilized by extensive hydrogen bonding. Crystal data ( 1): monoclinic, P2 1/c, a = 7.540(4), b = 12.954(4), c = 7.277(3) Å, β = 110.09(6), V = 667.4(5) Å 3, Z = 2, D calc = 1.955 Mg/m 3, μ = 2.079 mm -1, R = 0.0501 for [|I|≥2 (I)]. For ( 2): triclinic, P-1, a = 7.720(2), b = 7.916(2), c = 14.797(3) Å, α = 97.264(3), β = 104.788(3), γ = 105.171(3)°, V = 825.3(3) Å 3, Z = 2, D calc = 2.296 Mg/m 3, μ = 10.715 mm -1, R = 0.0308 for [|I|≥2 (I)]. For ( 3): monoclinic, P2 1/c, a = 7.595(3), b = 12.891(4), c = 7.204(3) Å, β = 111.07(3)°, V = 658.2 Å 3, Z = 2, D calc = 1.982 Mg/m 3, μ = 2.279 mm -1, R = 0.0552 for [|I|≥2 (I)]. For ( 4): monoclinic, P2 1/c, a = 7.840(2), b = 13.358(4), c = 7.518(2) Å, β = 110.923(3)°, V = 938.6(3) Å 3, Z = 2, D calc = 2.577 Mg/m 3, μ = 12.18 mm -1, R = 0.0280 for [|I|≥2 (I)]. For ( 5): orthorhombic, Pnma, a = 16.776(6), b = 11.943(4), c = 7.079(3) Å, V = 1418.2(9) Å 3, Z = 4, D calc = 2.564 Mg/m 3, μ = 12.639 mm -1, R = 0.0381 for [|I|≥2 σ(I)]. 相似文献
13.
Two new polyoxometalates [HN(C 2H 5) 3] 3[PMo 12O 40] ( 1) and [NH 2(C 2H 4NH 3) 2] 2[Mo 5P 2O 23] ( 2) have been hydrothermally synthesized and characterized by IR, UV-Vis, XPS spectra, TG analyses, and single crystal X-ray diffraction. Crystal data for 1: monoclinic, space group C2/ c, a = 24.651(5) Å, b = 10.822(2) Å, c = 22.413(5) Å, β = 120.37(3)°, and V = 5158.7(18) Å 3; for 2: triclinic, space group P-1, a = 9.821(2) Å, b = 9.948(2) Å, c = 14.687(3) Å, α = 95.490(3)°, β = 98.870(3)°, γ = 95.710(3)°, and V = 1401.7(5) Å 3. The crystal structure analyses reveal complex hydrogen bonds in both 1 and 2 in 3-D supramolecular arrays constructed from different polyoxoanions and organic ligands. 相似文献
14.
Two complexes with enoxacin and ciprofloxacin were synthesized and the crystal structures are reported. Compound 1, [Cu(H-Eno) · Cl 2] · 3H 2O (H-Eno = Enoxacin), crystallizes in the triclinic system, space group P 1, with lattice parameters a = 8.7731(12) Å, b = 9.4976(14) Å, c = 13.2033(19) Å, α = 86.319(7)°, β = 71.912(7)°, γ = 80.604(7)°, V = 1031.6(3) Å 3, Z = 2, D c = 1.625 mgm ?3. 2, [Mn(Cip) 2] · 2H 2O (Cip = mono-anion of ciprofloxacin), crystallizes in the monoclinic, space group P2( 1) /c, with lattice parameters a = 5.85690(10), b = 21.9490(6), c = 13.4443(3) Å, β = 100.9700(10)°, V = 1696.72(7) Å 3, Z = 2, D c = 1.459 mgm ?3. 相似文献
15.
Chemical preparation, crystal structure, thermogravimetric and differential analysis, solid state 31P MAS NMR characterization, and IR spectroscopic investigations are given for a new organic cation dihydrogenmonophosphate, (2-CH 3OC 6H 4CH 2NH 3)H 2PO 4. This compound is monoclinic C2/c, with unit cell parameters a = 27.740(8), b = 4.827(2), c = 16.435(3) Å, β = 93.79(2)°, V = 2196 (1) Å 3, Z = 8, and ρ = 1.422 g · cm ?3. The crystal structure has been determined and refined to R = 0.046 (Rw = 0.056), using 1,746 independent reflections with I > 3σ (I). Its atomic arrangement can be described by infinite polyanions [H 2PO 4] n n ?, organized in ribbons alternating with organic cations. Strong hydrogen bonds connect the different components. Electrical conductivity measurements show that the [2-CH 3OC 6H 4CH 2NH 3]H 2PO 4 has a low ionic conductivity value at 403 K. 相似文献
16.
Dimethylgallium-bis(trimethylsilyl)phosphane, Vibrational Spectrum, Force Constants, and X-Ray Structure Dimeric dimethylgallium-bis(trimethylsilyl)phosphane, [Me 2Ga? P(SiMe 3) 2] 2, (Me = CH 3) is synthesized from Me 2GaCl and P(SiMe 3) 3 in hot toluene. The compound crystallizes in the triclinic space group P1 with the cell parameters a = 909.8(2), b = 960.5(2), c = 971.6(2) pm; α = 76.75(1)°, β = 80.35(1)°, γ = 63.94(1)° and Z = 1 (dimer). The Ga? P distances are 244.8 and 245.2 pm, the ring angles are 91.8° (Ga? P? Ga) and 88.2° (P? Ga? P), respectively. The vibrational spectrum (IR and Raman for the solid) has been measured and assigned; force constants calculations are carried out for the skeleton [C 2Ga? P(SiC 3) 2] 2 using Fleischhauers [26] PC-program. 相似文献
17.
A dinuclear manganese(III) tetradentate Schiff-base complex, [Mn 2(salophen) 2(4,4′-bipy) 3](BPh 4) 2 ( 1) (salophen = N, N′- o-phenylene- bis(salicylideneaminato)), has been synthesized and structurally characterized. Compound 1 crystallized in the triclinic, P 1 space group, a = 13.431(4), b = 13.791(4), c = 13.886(4) Å, α = 73.599(5)°, β = 80.410(6)°, γ = 71.241(5)°, V = 2328.3(12) Å 3. Complex 1 contains two Mn(salophen) moieties bridged by 4,4′-bipy to form a dinuclear unit, with two terminal 4,4′-bipy ligands. Variable temperature magnetic susceptibility (2–300 K) shows very weak ferromagnetic interactions between the Mn(III) ions. 相似文献
18.
The alkylation of ethylenediamine with allyl bromide in the presence of a fourfold (with respect to ethylenediamine) molar
amount of NaHCO 3 in acetone with an ethanol admixture (15: 1) affords LBr 2 · 2H 2O ( I), where L 2+ is the N,N,N,N′,N′,N′-hexaallylethylenediaminium cation. Single crystals of complexes L[Cu II(Br 0.45Cl 3.55)] ( II), L[Cu 4I(Br 4.55Cl 1.45)] ( III), and L[Cu 4IBr 6] ( IV) are prepared by ac electrochemical synthesis from an ethanolic solution of LBr 2 · 2H 2O, CuCl 2 · 2H 2O (or CuBr 2) at copper wire electrodes. The crystal structures of compounds I–IV are determined by X-ray diffraction analysis. The crystals of complex I are monoclinic: space group P2 1/ n, a = 8.544(3), b = 10.404(3), c = 13.350(4) ?, β = 97.29(3)°, V = 1177.2(6) ? 3, Z = 2. The bromine anions in compound I are bonded to the L 2+ cations and water molecules through hydrogen contacts (E)H…Br (E = O, C) of 2.57(3)–2.86(3) ?. The crystals of compounds
II–IV are triclinic: space group P
. For II: a = 8.762(4), b = 9.163(4), c = 16.500(6) ?, α = 95.62(4)°, β = 96.39(4)°, γ = 111.46(4)°, V = 1211.4(9) ? 3, Z = 2; for III: a = 9.074(4), b = 9.435(4), c = 9.829(5) ?, α = 116.12(4)°, β = 104.14(4)°, γ = 100.22(4)°, V = 692.3(6) ? 3, Z = 1; for IV isostructural III: a = 9.084(4), b = 9.404(4), c = 9.869(4) ?, α = 116.31(3)°, β = 104.00(3)°, γ = 100.37(3)°, V = 692.1(5) ? 3, Z = 1. Unlike the isolated tetrahedral CuX 42− anion in structure II, an original chain anion (Cu 4X 62−)
n
is observed in the structures of π complexes III and IV.
Original Russian Text ? M.M. Monchak, A.V. Pavlyuk, V.V. Kinzhibalo, M.G. Mys’kiv, 2009, published in Koordinatsionnaya Khimiya,
2009, Vol. 35, No. 6, pp. 414–419. 相似文献
19.
The title compound was prepared by reaction of N, N‐dimethyldithiocarbamate sodium with l‐bromo‐l‐(4‐methoxyphenylcarbonyl)‐2‐(1, 2, 4‐triazole‐l‐yl) ethane. Its crystal structure has been determined by X‐ray diffraction analysis. The crystal belongs to triclinic with space group Pī, a = 0.7339(2) nm, b = 1.1032(2) nm, c = 1.1203(2) nm, a = 90.27(3)°, β = 102.03(3)°, γ = 104.91(3)°, Z=2, V = 0.8556(3) nm 3, Dc = 1.360 g/cm 3, μ =0.325 mm ?1, F(000)=368, final R1 =0.0475. The planes of 4‐methoxybenzyl group and triazole ring are nearly perpendicular to each other. The dihedral angle is 83.97°. There is an obvious π‐π stacking interaction between the molecules in the crystal lattice. The results of biological test show that the title compound has fungicidal and plant growth regulating activities. 相似文献
20.
Abstract Reactions of Mo(CO) 6 with Na 2WO 4 · 2H 2O in refluxing carboxylic anhydride produce the triangular bioxo-capped mixed-metal carboxylate clusters Na[MoW 2O 2(O 2CR) 9] (R = Me, 1; Et, 2), the propionate being hydrolyzed in 2M HCl containing ZnCl 2 to form [MoW 2O 2(O 2CEt) 6(H 2O) 3]ZnCl 4·2H 2O ( 3). Cluster 2 is converted to the incomplete cuboidal tetraanion [MoW 2O 4(O 2CEt) 8] 4- upon reacting with Cr(CO) 6 in propionic anhydride at 120°, the latter species being trapped by Cr 3± and Na ± ions in the reaction mixture to afford the octanuclear heterometallic chain-like cluster Na 2Cr 2 [MoW 2O 4(O 2CEt) 8] 2 ( 4). Clusters 1, 3 and 4 have been characterized by X-ray crystallography with the following crystal data, for 1: monoclinic, space group P2 1/ c, a = 16.666(8), b = 11.096(3), c = 16.541(7) Å, β = 94.60(4)°, V = 3048.9 Å 3, Z = 4, R, Rw = 0.070, 0.079; for 3, monoclinic, space group Cm, a = 10.259(3), b = 15.756(3), c = 10.870(3) Å, β = 96.18(3)°, V = 1746.8 Å 3, Z = 2, R, Rw = 0.028, 0.034; for 4, triclinic, space group P-1, a = 13.013(5), b = 14.005(4), c = 12.357(4) Å, α = 109.71(2), β = 117.77(3), γ = 90.41(3)°, V = 1838.9 Å 3, Z = 1, R, Rw = 0.037, 0.042. 相似文献
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