Crystal structures and vibrational spectra ofMSnF6·6H2O(M=Fe,Co, Ni)

Summary Single crystal X-ray structural data (atT=300 K) are reported for CoSnF₆·6H₂O (rhombohedral; R{ie61-1}-C _3i ² ;a=9.735(7) Å,c=10.095(7) Å, =120°;Z=3;R=0.047) and for NiSnF₆· 6H₂O (rhombohedral; R{ie61-2}-C _3i ² ;a=9.697(1)Å,c=10.021(1)Å, =120°;Z=3;R=0.038). The two compounds are isostructural to FeSnF₆·6H₂O. IR and Raman spectroscopic data (atT=300 and 75 K) are reported for hydrated and for partially deuterated samples ofMSnF₆·6H₂O (M=Fe, Co, Ni). Two rather similar (OD) stretching frequencies and one (HDO) bending frequency of isotopically dilute HDO molecules are observed for either of the three compounds, which is consistent with one crystallographically distinct water molecule forming two different, but rather similar O ... F hydrogen bonds.

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Kristallstrukturen und Schwingungsspektren vonMSnF₆·6H₂O (M=Fe, Co, Ni)

Zusammenfassung Die Kristallstrukturen von CoSnF₆·6H₂O (rhomboedrisch; R{ie61-3}-C _3i ² ;a=9.735(7) Å,c=10.095(7) Å, =120°;Z=3;R=0.047) und von NiSnF₆·6H₂O (rhomboedrisch; R{ie61-4}-C _3i ² ;a=9.697(1)Å,c=10.021(1)Å, =120°;Z=3;R=0.038) wurden mittels Röntgen-Einkristalldaten (beiT=300 K) bestimmt. Die beiden Verbindungen sind isostrukturell zu FeSnF₆·6H₂O. IR- und Raman-Spektren vonMSnF₆·6H₂O (M=Fe, Co, Ni) wurden von Proben mit unterschiedlichem Deuterierungsgrad gemessen (beiT=300 und 75 K). Bei allen drei Verbindungen findet man für isotopenverdünnte HDO Moleküle zwei nur geringfügig unterschiedliche (OD)-Valenzfrequenzen und eine (HDO)-Deformationsfrequenz, was mit der Existenz von nur einer Art von Wassermolekülen mit zwei verschiedenen, aber doch sehr ähnlichen O ... F Wasserstoffbrückenbindungen übereinstimmt.

     

Molecular and Crystal Structure of 2, 3, 5, 6-dipropylene-r-pyrone

11NTRODUCT1ONWeattemptedtosynthesizeanextractant(1)bythereactionofadipylchloridewithcyclopentanonepiperidineenamineaccordingtoHunig'sprocedure"',however,wemainlyobtainedthetitlecompound,whichmaybepossiblyapotentialmedicinet2'3i.Itsmolecularstructurewasfinallyconfirmedbythesingle-crystalstructuredeterminationafterconventionalUV,IR,lHNMR,MSandelementana-lyticalworks.2EXPER1MENTALSECT1ON2.1SynthesisToastirredsolutioncontaining8Omlofchloroform,2.8mloftri-ethylamineand1.51g(O-Olmol)…     

Synthesis and Crystal Structure of N, N'''''''',N''''''''-Tris-(2-oxynaphthalidene)-tris-(2-iminoethyl) Amine

1 INTRODUCTION Schiff’s bases are well known ligands representedby many bi-, tri-, tetra-, and hexa-dentate example-es[1], but heptadentate ligands are relatively rare[2, . 3]We have reported a copper complex of tetradentateSchiff’s bases[4]…     

Crystal growth, structural, thermal, and dielectric characterization of Tutton salt (NH4)2Fe(SO4)2·6H2O crystals

A good quality single crystal of Tutton salt, (NH₄)₂Fe(SO₄)₂·6H₂O, with dimensions 6 × 7 × 3 mm³ was successfully grown by the slow evaporation growth technique at ambient temperature. The grown crystal was subjected to single crystal X-ray diffraction study which confirms that the grown crystal is monoclinic in nature with the space group P2₁/c. Optical absorption spectrum reveals that the grown crystal has good optical transparency in the entire visible region and its energy band gap was determined. The thermal behavior of the grown crystal was investigated by thermogravimetric and differential thermal analysis. The dielectric measurements were carried out to determine the dielectric behavior of the crystal.     

Synthesis,Characterization and Crystal Structure of (PhCH2)2Sn(S2CENt2) and (PhCH2)2Sn(S2CNC4H8)2

Two new dibenzyltin bisditiocarbamates(PhCH2)2 Sn(S2CNEt2)2(1) and (PhCH2)2 Sn(S2CNC4H8)2(2) were synthesized by the reaction of dibenzyltin dichloride with dithiocarbamates and characterized by elemental analysis ,IR,^1H NMR and MS spectra.The crystal structures were determined by X-ray single crystal diffraction analysis.In both complexes,the tin atom is six-coordinated in a distorted octahedral configuration.In the crystals of 1,the molecular packing in unit cell reveals that the two adjacent molecules are symmetrically linked to each other in dimers by two Sn S interactions of 0.3816nm.In the crystals of 2,the molecules are packed in the unit cell in one-dimensional chain structure linked by weaker intermolecular S S conmtacts.     

Crystal structure of CsLnFe(CN)6·5H2O (Ln=Ce,Pr, Nd), CsCeFe(CN)6·4H2O,and TlTmRu(CN)6·3H2O

We have investigated the crystal structures of CsLnFe(CN)₆·nH₂O (Ln=lanthanide, n=4,5), as well as TlTmRu(CN)₆·3H₂O. These phases can be thought of as derivatives of LnFe(CN)₆·4H₂O, where, simultaneously, an alkali ion (or Tl⁺) is introduced while the valence of Fe is reduced from Fe³⁺ to Fe²⁺. A new arrangement of the structural units is observed in the CsLnFe(CN)₆·5H₂O, where the coordination of the Ln-ion is changed to a bisdisphenoid. The resulting LnN₅O₃ units alternate with Fe(CN)₆ units to form an overall rocksalt-type ralted lattice that accommodates the alkali ions in interstitial sites. Due to the arrangement of the water molecules, a layer structure results.     

Syntheses, Crystal Structures and Photoluminescence Properties of Cadmium(Ⅱ) and Nickel(Ⅱ) Complexes with 2-(2-Benzimidazolyl)quinoline

Two novel complexes, [Cd2(BMQU)2Cl4] (1) and [Ni(BMQU)2HPO4]·1.5H2O (2) (BMQU = 2-(2-benzimidazolyl)quinoline), were synthesized by the hydrothermal method and characterized by elemental analysis, IR, and TG-DTG. The crystal structures were determined by single-crystal X-ray diffraction. Both 1 and 2 crystallize in the triclinic system, space group P . The data for 1: a = 0.8342(7), b = 0.9226(9), c = 1.0646(8) nm, α = 90.819(2), β = 97.466(2), γ = 98.280(2)°. The Cd(Ⅱ) is coordinated with three chlorine atoms and two nitrogen atoms of a BMQU molecule, generating a distorted square-pyramidal geometry. The dinuclear Cd(Ⅱ) complex is formed by two chlorine bridge bonds, and the one-dimensional chain structure is constructed with the hydrogen bond N-H…Cl and π-π stacking interaction. The data for 2: a = 1.2251(1), b = 1.2451(1), c = 1.2868(1) nm, α = 107.510(2), β = 98.630(1), γ = 109.921(2)°. The Ni(Ⅱ) is coordinated with four nitrogen atoms of two BMQU molecules and two oxygen atoms of a HPO42-, forming a distorted-octahedral geometry. The two-dimensional layer structure is formed by the hydrogen bonds and π-π stacking interaction between neighboring molecules. Complex 1 shows a strong blue fluorescence emission (λmax= 456 nm) at solid state.     

Synthesis and Crystal Structure of a Cyano-bridged Bimetallic Complex [La(betaine)2(H2O)6Fe(CN)6]·2H2O

The title complex [La(betaine)2(H2O)6Fe(CN)6](2H2O (betaine = (CH3)3NCH2CO2) has been synthesized and characterized by X-ray single-crystal structure analysis. The crystal crystallizes in monoclinic, space group P21/n with a = 15.793(5), b = 8.927(3), c = 22.257(7) (A), β = 110.147(5)°, C16H38FeLaN8O12, Mr = 729.31, Z = 4, V = 2946.0(15) (A)3, Dc = 1.640 g/m3, μ(MoKα) = 1.988 mm-1, F(000) =1476, R = 0.0388 and wR = 0.0827 for 4237 observed reflections (I > 2σ(I)). The La3+ ion is nine-coordinated by one cyano nitrogen atom and eight oxygen atoms of two betaine and six water molecules. Each complex molecule is connected to form a 3D network structure by some O-H…O and O-H…N hydrogen bonds.     

Synthesis,Crystal Structure and Evaluations of Its Cytotoxicity,Anti-microbial and Anti-hydroxyl Radical Activities of a New Co-crystal Compound(C_6H_6Cl_2N_2O_2S)·(Phen)·H_2O

Co-crystal is a very potential kind of drug solid forms, and has a far-reaching influence on designing and preparing drugs. A new 1:1:1 co-crystal compound consisting of 4-amino-3,5-dichloro-benzenesulfonamide, 1,10-phenanthroline and water was synthesized, and its crystal structure was characterized by X-ray diffraction method. The compositions of the co-crystal are self-assembled into a three-dimensional network structure via intermolecular interactions including hydrogen bonds, π-π stacking, Cl???Cl interactions and van der Waals' forces. According to the evaluations of cytotoxicity assays, anti-microbial and anti-hydroxyl radicals, this co-crystal is a potential drug.     

Syntheses and Crystal Structures of Sm(OAr)2(THF)3·THF and Sm(OAr)2(DME)2 (Ar = C6H2-tert-Bu3-2,4,6)

Reaction of SmI2(THF)x with 2 equivalents of NaOAr (Ar = C6H2-tert-Bu3-2,4,6)1,2-dimethoxyethane (DME) leads to the ligand-exchange reaction, and a DME-solvated complex of Sm(Oar)2(DME)2 2 was obtained. Complex 1 crystallizes in monoclinic, space group P21/c with a =10.366(5), b = 33.024(15), c = 16.123(7) (A), β= 93.197(8)°, V= 5511(4) A3, Z= 4, C52H9oO6Sm, Mr = 961.59, Dc = 1.159 g/cm3, F(000) = 2048,μ(MoKα) = 1.107 mm-1, R = 0.0844 and wR = 0.1401for 4694 observed reflections. Complex 2 crystallizes in monoclinic, space group C2/c with a =27.222(5), b = 10.6140(19), c = 17.398(4) (A), β = 110.245(3)°, V = 4716.4(16) (A)3, Z = 4,C44H78O6Sm, Mr = 853.41, Dc = 1.202 g/cm3, F(000) = 1808,μ(MoKα) = 1.285 mm-1, R = 0.0361and wR = 0.0830 for 5210 observed reflections.     

Synthesis, Dimeric Crystal Structure, and Biological Activities of N-(4-Methyl-6-oxo-1,6-dihydro-pyrimidin-2-yl)-N′-(2-trifluoromethyl-phenyl)-guanidine

IntroductionPlants have a more extensive biosynthetic capacitythan animals, which is attributed to the fact that ani-mals rely on their diet for the supply of many biochemi-cal compounds and their precursors. Owing to thisdifference, plants contain numero…     

The Crystal and Molecular Structure of a New Macrocyclic Ligand, (H_6BDBPH)Br_6·4H_2O

1　ＩＮＴＲＯＤＵＣＴＩＯＮＯｎｅｏｆｏｕｒｃｕｒｒｅｎｔｉｎｔｅｒｅｓｔｓｆｏｃｕｓｅｓｏｎｔｈｅｄｅｓｉｇｎａｎｄｓｙｎｔｈｅｓｅｓｏｆｐｏｌｙａｚａｍａｃｒｏｃｙｃｌｉｃｌｉｇａｎｄｓ,ａｎｄｔｈｅｓｔａｂｉｌｉｔｉｅｓｏｆｃｏｒｒｅｓｐｏｎｄｉｎｇｍｅｔａｌｃｏｍｐｌｅｘｅｓ.Ｔｗｏｐｏｌｙａｚａｄｉｐｈｅｎｏｌｍａｃｒｏｃｙｃｌｅｓ,Ｒ(ｂａｂｐ) 2 (ｄｆｃ) 2 ａｎｄＲ (ｂａｃ) 2 (ｄｆｐ) 2 ;[1 ]ｏｎｅｏｃｔａａｚａ ｍａｃｒｏｃｙｃｌｅ,ＢＰＢＤ ;[2 ,3]ａｎｄｓｅｖｅｒａｌｈｅｘａａｚａｍａ…     

Synthesis and Crystal Structure of Compound 〔ZnS_6(C_(12)H_8N_2)〕

１　ＩＮＴＲＯＤＵＣＴＩＯＮＩｎｒｅｃｅｎｔｙｅａｒｓ,ｔｈｅｚｉｎｉｃｃｏｍｐｏｕｎｄｓｃｏｎｔａｉｎｉｎｇｓｕｌｆｕｒａｎｄｎｉｔｒｏｇｅｎａｔｔｒａｃｔｍｏｒｅａｎｄｍｏｒｅａｔｔｅｎｔｉｏｎｂｅｃａｕｓｅｏｆｔｈｅｉｒｄｅｅｐｒｅｌａｔｉｏｎｓｈｉｐｗｉｔｈｂｉｏ－ｉｎｏｒｇａｎｉｃｃｈｅｍｉｓｔｒｙ〔１〕．Ｚｉｎｉｃｓｕｌｆｉｄｅｐｌａｙｓａｎｉｍｐｏｒｔａｎｔｒｏｌｅｄｕｅｔｏｉｔｓｓｉｇｎｉｆｉｃａｎｔｉｎｖｏｌｖｅｍｅｎｔｉｎｔｈｅｓｔｕｄｙｏｆｔｈｅｐｈｏｓｐｈｏｒｓ,ｓｅｍｉ…     

Synthesis and Crystal Structure of 2-Nitrophenyl N,N-Bis(2-chloroethyl)-N'-(4-methylbenzene- sulfonamino)ethyl-phosphorodiamidate

1 INTRODUCTION Nitrogen mustards (NMs) are useful chemothe- rapeutic agents in the treatment of lymphoma, leuke- mia, multiple myeloma and ovarian carcinoma[1]. The antitumor activity of NMs has been attributed to their ability to cross-link the twin strands of DNA. Phosphoramide mustard is also an alkating agent that cross-links interstrand DNA, such as cyclophos- phamide (CP) , ifosfamide (IFA) and trofosf- amide[2～5]. Cyclophosphamide is a widely used anticancer alklating agent …     

Growth and Optical Properties of Sr_6YbSc(BO_3)_6 Crystal

1INTRODUCTION As is well known,the Yb3 ion has some advan-tages in comparison with Nd3 as laser active ion,for it has only two manifolds,i.e.,the ground2F7/2state and the excited2F5/2state.There is no excited state absorption reducing effective laser cross-section,no concentration quenching,no up-conversion,and three or four times longer emission lifetime than Nd3 ion.Yb3 ion exhibits a strong and broad ab-sorption band at ca.970nm and can be easily pumped with InGaAs diode lasers.The …     

Synthesis, Characterization, Crystal Structure and Antibacterial Activities of a Nickel(Ⅱ) Complex with 2'-(2-Thienylidene)-hydroxybenzoylhydrazide

In the ethanol solvent, a nickel(II) complex Ni(C12H10N2O2S)2 upon reaction of 2'-(2-thienylidene)-hydroxybenzoylhydrazide with nickel acetate was synthesized, and its structure was characterized by IR, UV, elemental analysis and X-ray diffraction analysis. The crystal belongs to monoclinic system, space group C2/c with a = 22.052(3), b = 5.9681(6), c = 18.522(2) , β = 110.679(4)°, V = 2280.6(4) 3, Z = 4, Mr = 551.27, μ = 1.606 mm-1, Dc = 1.075 g/cm3, F(000) = 1136 and Rint = 0.0556. The nickel(Ⅱ ) atom in the compound is four-coordinated with two nitrogen atoms from amide and two oxygen atoms from keto group. The biological activities have been measured, show- ing the compound exhibits better anti-bacterial activity than the ligand.     

Synthesis and Crystal Structure of Ni_3(admt)_6(NCS)_6·C_2H_5OH·2H_2O

1　INTRODUCTIONCoordination compounds with 1 ,2 ,4 triazole as a ligand have interesting fea tures,notonly because ofthe very interesting magnetic propertiesofthese complex es,but also because ofrich modes ofcoordination〔1〕.Particularly,the coordinationbehavioroftriazoletowardsa numberoftransition metalthiocyanatesshowsremark abledifferences〔2 - 6〕.On unsubstitution at N4 ,thetriazole ring hasmonodentate,1 ,2 and 2 ,4 bridging forms.These three modes were all observed in the Ni( II)…     

Growth and Characterization of Crystal Nd_(0.06)Y_(0.94)Sr_6Sc(BO_3)_6

<正>The crystal of Nd0.06Y0.94Sr6Sc(BO3)6 with the dimensions up to 35 mm × 28 mm × 13 mm was grown by a top-seeded solution growth method from Li6B4O9 flux. The grown crystal was characterized by X-ray powder diffraction. The optical absorption of the crystal shows that it has a strong absorption band at 8070 A, and the absorption coefficient is 2.17cm-1 with a FWHM of 41 A, which can match with the wavelength of the diode-laser (LD) and is suitable for the LD pumping. Based on the Judd-Ofelt theory, the three parameters of line oscillator strength Ω(λ) (λ = 2, 4 and 6) of the Nd3+ion in the crystal were calculated as follows: Ω2= 1.194 × 10-20, Ω4= 4.186 × 10-20 and Ω6 = 3.351 × 10-20cm2, which are relatively larger. The results indicate that the crystal Nd0.06Y0.94Sr6Sc(BO3)6 may be a kind of high-efficient laser material for diode-pumped.     

Synthesis, Crystal Structure of Co(Ⅱ)(6-methoxybenzothiazole-2-carboxylate)_2(DMF)_2 and Its Application to Carbonylation of Benzyl Chloride

A new complex, Co(MBTC)₂(DMF)₂ (MBTC=6‐methoxybenzothiazole‐2‐carboxylate, DMF=N,N‐dime‐ thylformamide), was synthesized in DMF solution and characterized by single crystal X‐ray diffraction analysis. Using the cobalt complex as catalyst, phenylacetic acid was prepared by the carbonylation of benzyl chloride with carbon monoxide (0.1 MPa). The effects of solvents, phase transfer catalysts and temperature on the reactions were investigated. The yield of phenylacetic acid was higher than 90% in optimized condition.     

Crystal Structure of (Hg, Ce, Cu)(Sr, Pr)2(Pr, Sr)Cu2O6+δ and (Hg, \square )(Sr, Pr)2(Pr, Sr)2Cu3O8+δ Phases

This paper reports on the refined compositions and crystal structures of two phases from the homologous series (Hg, M)(Sr, Pr)₂(Pr, Sr)_k-1Cu_kO_2k+2+ with k = 2 (Hg-1212) — (Hg_0.44(2)Ce _0.31 ⁴⁺ Cu_0.25)(Sr_0.90(3)Pr_0.10)₂(Pr_0.52(3)Sr_0.48)Cu_2.00O_7.00 (a = 3.8634(1), c = 12.2030(8) , space group P4/mmm) with k = 3 (Hg-1223) — (Hg_0.29(1) )(Sr_0.67(2)Pr_0.33)₂(Pr_0.61(2)Sr_0.39)₂Cu_3.00O_9.32(8) or (Hg_0.29(1) )(Sr_0.61(4)Pr_0.39)₂(Pr_0.51(4)Sr_0.49)₂Cu_3.00O_9.00 (with a fixed content of superstoichiometric oxygen O(4) in the phase) ( is a vacancy; a = 3.8294(9), b = 3.8567(6), c = 15.2763(44) , space group Pmmm). The implausibly high content of oxygen in the Hg-1223 phase (refinement I) is attributed either to O–O bond formation or to the possible presence of a minor amount of copper in a defect position of Hg; the inclusion of the latter in structure refinement leads to a better reproduction of the real structure but increases the R indices. The crystal-chemical analysis of the title phases and a comparison with the available data for analogous phases indicates that the composition of the crystallographic positions is related to structural features, in particular, to the coordinates of (Hg, M) and superstoichiometric oxygen, whose content depends on the degree of substitution of strontium ions by praseodymium ions. Reasons for the orthorhombic distortion of the Hg-1223 phase are discussed. The absence of superconductivity is explained by the nonoptimal formal charge (FC) of copper, which depends on the oxygen content in the phase.