Crystal Structure and Luminescence of 1,10-Phenanthroline-tris(4-methoxybenzoato)Europium

1,10 Phenanthroline tris(4 methoxybenzoate)europium, Eu( p MOBA) 3phen(where p MOBA= p methoxybenzoate and phen=1,10 phenanthroline) has been obtained in the ethanol solution. The crystal consists of binuclear molecules of the title compound. In the binuclear molecule each Eu 3+ ion is coordinated not only by four oxygen atoms from the bridging carboxylates, but also by two oxygen atoms of a bidentate carboxyl group and two nitrogen atoms of a phen chelating ligand, giving coordination number of eight. Eu O distances range from 0 2336(3) to 0 2483(3) nm. The average Eu N distance is 0 2624(4) nm. Luminescence data indicate that one Eu 3+ ion site is in low symmetry in the complex.

Synthesis and Crystal Structure of α-( N-Protected a mino)β-lactam Derivative of 1 ,5-Benzothiazepine

The crystal of the title compound C, C 30 H 30 N 2O 3S has been prepared by reaction of 1,5 benzothiazepine with N protected glycine and determined by X ray single crystal diffraction. Crystal data: M r =498.62, triclinic with P 1 space group, a=10.880(2), b=13.955(3), c=9.537(2), α=99.34(3)°, β=110.43(3)°, γ=88 56(3)°, V=1338.2(5) 3, F(000)=528, λ (Mo Kα)=0.71073, Z=2, D c =1 237g/cm 3, μ =0.154mm -1 . Final R=0.0453, wR =0.1256 for 3491 observed reflections 〔 I>2σ(I) 〕. Structure analysis reveals that the substituents at C(23) and C(7) in four membered ring are located on the same side. The conformation of seven membered ring is chair like.

Syntheses and Crystal Structures of Pyrazoline Derivants

Two pyrazoline derivants 1-(2-benzothiazole)-3-phenyl-5-(3-thiophene)-2- pyrazoline (BPTP) and 1-(2-benzothiazole)-3-(2-thiophene)-5-phenyl-2-pyrazoline (BTPP) have been synthe- sized and their crystal structures were determined by X-ray single-crystal diffraction. Crystal of BPTP belongs to triclinic, space group P1 with a = 9.4430(11), b = 9.9384(13), c = 9.9394(13) ?, α = 83.107(10), β = 79.947(10), γ = 70.221(7)o, V = 862.42(19) ?3, Z = 2, Dc = 1.392 g/cm3, μ(MoKα) = 0.316 mm-1, F(000) = 376, λ = 0.71070 ?, (?ρ)max = 0.348, (?ρ)min = –0.481 e/?3, the final R = 0.0407 and wR = 0.1055 for 2844 observed reflections with I > 2σ(I). Crystal of BTPP is of monoclinic, space group P21/c with a = 11.6158(17), b = 11.2796(18), c = 13.082(2) ?, α = 90, β = 91.087(4), γ = 90o, V = 1713.7(5) ?3, Z = 4, Dc = 1.401 g/cm3, μ(MoKα) = 0.318 mm-1, Mr = 361.07, F(000) = 752, λ = 0.71070 ?, (?ρ)max = 0.322, (?ρ)min = –0.330 e/?3, the final R = 0.0563 and wR = 0.1058 for 3434 observed reflections with I > 2σ(I).

Crystal Structure of RbYbI_3

The crystal structure of RbYBI 3 is determined by X ray powder diffraction method, and its crystal structure is refined by Rietveld technique Its crystal structure is orthorhombic system with a =1 0383(3) nm, b =0 4667(1) nm, c =1 7200(5) nm The space group is Pnma (62), Z =4, and all of the atoms occupy the 4 c positions of the Pnma space group Each Yb atom is coordinated by six I atoms to form a distorted octahedron The main feature of the crystal structure of RbYbI 3 is two chains along the b axis which are composed of the edge sharing octahedra

Synthesis and Crystal Structure of Europium Associate(C34H54N2O10)[Eu（NO3）5]

The title compound, (C 34 H 54 N 2O 10 )[Eu(NO 3) 5](C 34 H 52 N 2O 10 =1,2 bis(2,3 benzo 10 aza 15 crown 5 N ethyleneoxy)ethane), was synthesized in acetonitrile solution and its crystal structure was determined by X ray analysis. The crystal crystallizes in monoclinic, space group P21/c with cell parameters a =1 1801(2) nm, b =2 3560(5) nm, c =1 7025(3) nm, β =99 67(3)°, V =4 6662(16) nm 3, Z =4, D c=1 581 g/cm 3. The europium ion is coordinated with ten oxygen atoms from five nitrato groups, and neither O atoms nor N atoms of the macrocyclic compound are bonded to the europium ion.

Synthesis and Crystal Structure of Quaternary Mixed Anion Complexes of Lanthanide Containing 1,10-Phenanthroline

A series of novel quaternary mixed anion complexes of lanthanide containing 1,10 phenanthroline(phen) were synthesized from the water/ethanol solution with slightly acidic solution and characterized by elemental analysis, IR and UV spectra, thermal analysis and single crystal X ray diffraction analysis. The crystal of [Ce(CH 3COO) 2(NO 3)(phen)] 2 belongs to monoclinic system, lattice type C centered, space group C 2/m, a =1 5444(6) nm, b =1 2273(5) nm, c =1 2776(5) nm, β =131 89(2)°, V =1 802(1) nm 3, Z =2, R =0 024, R w =0 032.

Synthesis and Crystal Structure of an Erbium Complex with Valine [Er_2(Val)_4(H_2O)_8](ClO_4)_6·4H_2O

The title complex was synthesized in aqueous solution, and its crystal structure was determined by X ray diffraction. The crystal is triclinic space group P 1 with a =1 00935(9) nm, b =1 20190(2) nm, c =1 28432(8) nm, α =95 013(9)°, β =102 814(5)°, γ =113 368(9)°, V =1 3676(3) nm 3, Z =1, D c=1 962 g/cm 3. The complex is a dimeric molecule with four bridging carboxyl groups from four valine molecules between two erbium ions. Each erbium ion is coordinated by four oxygen atoms from four carboxyl groups and four oxygen atoms of four water molecules with the coordination number 8, taking a square antiprism arrangement.

Synthesis and Crystal Structure of [Er(OH_2)_8](ClO_4)·3·5(1,4Diox.)·2H_2O

The title complex was synthesized in aqueous solution, and its crystal structure was determined by X ray diffraction. The crystal is monoclinic, space group P2 1/n with a =1 1243(3) nm, b =2 4853(2) nm, c =1 2962(1) nm, β =95 08(1)°, V =3 608(1) nm 3, Z =4, D c=1 757 g/cm 3. Each of the erbium ion is coordinated by eight water molecules. The complex is of polymeric structure with the octaaqua erbium complex species connected by 1,4 dioxane moieties through hydrogen bonds.

Synthesis and Crystal Structure of Tl[（C2H5O）2PS2]

The complex crystal of Tl[(C 2H 5O) 2PS 2] synthesized by thallous sulfate and di (2 ethyl) dithiophosphato (L) belongs to monoclinic system, space group P2 1/C. The cell parameters are: a =1 2245(4) nm, b =0.7195(3) nm, c =1.2327(4) nm, β =110.06(3), the volume V =1.020(1) nm 3, the molecular number in a cell Z =4, the density D x=1.622 kg·m -3 ; the structure factor F (000)=508 e, R factor R =0.068. The Tl(I) ion coordinates with two sulfur atoms of complexant L, and formes a frog like molecular configuration. The thermal stability of Tl[(C 2H 5O) 2PS 2] complex is attested by TG DTA and MS analysis.

Crystal Structure and X-ray Powder Diffraction Data for Rare Earth Compound PrNiSn

The compound PrNiSn was studied by X ray powder diffraction technique. The crystal structure and the X ray diffraction data for this compound at room temperature were reported. The compound PrNiSn is orthorhombic with lattice parameters a =0.74569(3) nm, b =0.76851(5) nm, c =0.45676(8) nm, V =0.26176 nm 3, Z =4 and D x=8.076 g·cm -3 , space group Pna2 1(33). The figure of merit F N for the compound is F 30 =54 (0.0093, 60).

Synthesis and Crystal Structure of a Two-dimensional Polymeric Holmium Complex〔Ho（H2saln）1.5（NO3）3〕

The title polymeric complex Ho(H 2saln) 1.5 (NO 3) 3 (H 2saln= N,N’ bissalicyclidene ethylenediamine) C 24 H 24 N 6O 12 Ho was prepared and its crystal was characterized by X ray diffraction. The ligand is dischiff base from salicylaldehyde and ethylenediamine. The complex crystallizes in trigonal system, space group P3c1 (No. 165), M r=753.42, a=15.818(2), c=16.978(3) , V=3681(2) 3, D x =1.360 g/cm 3, Z=4, μ =2.2286 mm -1 , F(000)=1492, R=0.049, R w =0.061. In the complex the coordination number of Ho(Ⅲ) is 9 with the geometry of a tricapped trigonal prism. All of the coordination atoms are oxygen atoms. The Ho(Ⅲ) ions are bridged by the dischiff base to form an infinite two dimensional polymeric network, parellel to the (001) plane.

Synthesis and Crystal Structure of 10-Phenyl-1,7-dithia-4-oxa-10-aza-12-crown-4

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Crystal Structure of 2-〔(P,P-Diphenoxy)phosphono(p-methyl)benzyl〕-1,2-benzisoselenazol-3(2H)-one

The crystal structure of the title compound 2 (P, P Diphenoxy)phosphono( p methyl)benzyl 1, 2 benzisoselenazol 3 (2H) one, C 27 H 22 NO 4PSe, was determined by single crystal X ray diffraction. It crystallizes in the triclinic system, space group P1 (No. 2) with M r=534.41, a=9.761(2), b=10.304(2), c=13.396(3) , α=110.97(3), β=107.70(3). γ=90.02(3)°, V=1190(1) 3, Z=2, D x =1.492 g/cm 3 , λ=0.71073 , μ =1.6596 mm 1 and F(000)=544. The structure was solved by direct methods. The final R factor is 0.068 and R w is 0.074 for 2500 unique observed reflections I≥3σ(I) . The results presented herein indicate that the selenium containing bicyclic moiety is a coplanar structure and that two adjacent molecules are symmetrically linked to each other forming a dimer through the Se(1c)…O=P(1) bonding interaction with an intermolecular Se(1c)…O distance of 2.797 .

The Crystal Structure of Biphenyltetracarboxylic Dianhydride Isomers

Biphenyltetracarboxylic dianhydride (2,2',3,3' BPDA), C 16 H 6O 6, M r =294.21, monoclinic, P2 1/c, a=11.694(2), b=8.111(2), c=13 494(3) , β=103.47(3)°, V=1244.7(4) 3, Z=4, D c =1.570 g/cm 3 , F (000)=450, Mo Kα radiation( λ =0.71073), μ (Mo Kα )=0.092 mm -1 , R =0.0329 for 2180 observed reflections 〔 I>2σ(I) 〕. 3,3',4,4' Biphenyltetracarboxylic dianhydride (3,3',4,4' BPDA), C 16 H 6O 6, M r =294.21, monoclinic, P2 1/n, a=6.8720(14), b=5.1870(10), c=17.288(4), β=94.96(3)°, V= 613.9(2) 3, Z=2, D c =1 592 gcm -3 , F(000)=300 , μ (Mo Kα )=0.125mm -1 , R =0.0331 for 1079 observed reflections〔 I>2σ(I) 〕. The dianhydride isomers have different symmetry caused by alternating two anhydride group positions and the dihedral angle between the two phenyl rings are 62.9°for 2,2',3,3', BPDA and 0°for 3,3',4,4' BPDA respectively.

Synthesis and Crystal Structure of 〔EDA〕〔Ni（dmit）2〕3

The crystal structure of the compound EDA Ni(dmit) 2 3 (EDA=2 diethylamino 1,3 dithioanylium; dmit=1,3 dithiole 2 thione 4,5 dithiolate)C 25 H 14 NNi 3S 32 , has been determined by single crystal X ray diffraction at 300K. The crystal is triclinic with space group P1, a=11.252, b=12.192(2), c=20.055(6) , α=108.127(2), β=106.287(8), γ=90.005(9)°; V=2498.3(3) 3, Z=2, M r=1530.38, D c =2.03(2) g/cm 3. Final R and R w values were 0.0603 and 0.0704, respectively. The structure consists of thick layers of stacked Ni(dmit) 2 entities separated by EDA cations. This salt shows semiconducting behaviour with room temperature conductivity of 0.2 Scm -1 and activation energy of 0.11 eV.

Hydrothermal Synthesis and Crystal Structure of a Keggin Polyoxometalate [Co^Ⅱ（2,2′-bipy）2（H2O）]2[SiW^Ⅵ12O40]·2H2O

A Keggin-type tungstosilicate compound [Co^Ⅱ（2,2′-bipy）2（H2O）]2[SiW^Ⅵ12O40]·2H2O 1 （bipy = bipyridine） was prepared by a hydrothermal method for the first time. Single-crystal X-ray diffraction revealed that 1 （C40H40Co2N8O44SiW12） crystallizes in the triclinic system, space group P1 with a = 10.4979（6）, b = 13.3946（7）, c = 13.5756（8）A, α= 70.0769（18）, β = 68.910（3）, γ = 74.186（4）°, V = 1649.84（16）A^3, Mr = 3688.95, Z = 1, Dc = 3.713 mg·m^-3, μ = 21.432 mm^-1, F（000） = 1644, S = 1.058, the final R = 0.0511 and wR =0.1023 for 6523 observed reflections （I 〉 2σ（I））. Compound 1 consists of two coordinated cation fragments [Co^Ⅱ（2,2′-bipy）2（H2O）]^2＋, one normal Keggin polyanion unit [SiW^Ⅵ12O40]^4- and two lattice water molecules. To be noted, each polyanion unit is linked to two cation fragments by its two surface terminal oxygen atoms and two cobalt atoms of two cation fragments forming an organic-inorganic hybrid unit in 1. Furthermore, the compound shows strong photoluminescence property in the solid state at room temperature.

Crystal Structure of cis-2-〔(P,P-Diethoxy)phosphono(m-nitro)benzyloxy〕-4-Phenyl-5,5-Dimethyl-1,3,2-Dioxaphosphorinane 2-Sulfide

The crystal structure of the title compound cis 2 (P, P Diethoxy)phosphono( m nitro)benzyloxy 4 Phenyl 5,5 Dimethyl 1,3,2 Dioxaphosphorinane 2 Sulfide, C 22 H 29 NO 8P 2S, was determined by single crystal X ray diffraction. It crystallizes in the monoclinic system, space group P2 1/c, with M r=529.49, a=9.888(2), b=20.831(4), c=12.797(3) , β=94.42(3)°, V=2628(1) 3, Z=4, D x =1.338 g/cm 3 , λ=0.71073 , μ =0.2796 mm 1 and F(000) =556. The structure was solved by direct methods. The final R factor is 0.052 and R w is 0.057 for 1793 unique observed reflections I≥3σ(I) . A cis configuration and a preferred chair conformation for the molecule have been established by X ray diffraction analysis. The results presented also give a good explanation to the correlation between the configurational assignments and the regularity in the chemical shifts of C 4-H and 31 P NMR.

Synthesis and Crystal Structure of ｛( P Ph_3)_2 Cl Ru( μ- Cl) Ru( P Ph_3) B_(10)H_7〔 O C H( C H_3)_2〕_3｝·0 .4( H_2O)

The title compound has been synthesized by the reaction of 〔RuCl 2(PPh 3) 3〕 and closo 〔B 10 H 10 〕 2- in (CH 3) 2CHOH solution. Crystals suitable for a single crystal X ray diffraction analysis were obtained from n pentane diffused to CH 2Cl 2 solution. The crystal {(PPh 3) 2ClRu( μ Cl)Ru(PPh 3)B 10 H 7〔OCH(CH 3) 2〕 3}·0.4(H 2O) is monoclinic , space group P2 1/n , M r= 1359.47, with a=19.434(4), b =14.340(4), c=25.865(9) , β= 95.48(3)°, V=7175(4) 3, D c =1.258 g/cm 3, Z=4, λ (Mo Kα )=0.71073, μ=6.03 cm -1 , F(000)=2784, R=0.0631, wR 2 = 0.1425, S =1.001. The title compound is a bimetallic species in which the second ruthenium center is bound to the cluster {(PPh 3)RuB 10 H 7〔OCH(CH 3) 2〕 3} via an Ru-Cl-Ru and two Ru-H-B-Ru bridges. The third isoproxy group replaces a hydrogen atom on B(10) of the cage, which indicates the activity of the cage.

Synthesis and Crystal Structure of Binuclear Complex of Copper(Ⅱ)Chloroacetate with Acetamine

The title complex, Cu 2(O 2CCH 2Cl) 4 OC(NH 2)CH 3 2, crystallizes in space group P2 1/a with a=7.616(4), b=18.665(5), c=7.949(5) , β=106.29(5)°. V=1084(1) 3, Z=2, M r=619.19, D c =1.896 g/cm 3; μ =25.05 cm -1 and F(000)=620.00, R =0.045 and R w =0.054 for 1807 observable reflections. X ray crystal structure analysis revealed that two Cu atoms are bridged by four chloroacetate groups, and the acetamine ligands are bonded by O(carboxide) to the terminal Cu atoms of each dimeric unit. The coordination geometry of Cu atom is a distorted octahedral configuration. The distance between the two Cu atoms is 2.648(1) .

Crystal Structure of Mixed Sodium-Potassium Paradodecatungstate 6-Hydrate

The crystal structure of K7Na3H2W12O426H2O was determined by Xray crystallography and refined to R=0.0864 based on 7024 observed reflections (I>2(I)). The crystallographic parameters are a=11.755(2), b=13.0493(3), c=16.289(3); =77.13(3), =82.92(3), =89.65(3), triclinic, space group, P1 , V=2416.7(8)3, Z=2, Mr=3330.98, Dcal=4.578Mg/m3, F(000)=2904, (MoK)=29.170mm-1, T=293K. Two independent polyanions are centered respectively at 1,1,1/2 and 1/2, 1/2, 0, approximately perpendicular to each other with dihedral angle between the equatorial planes of the molecules at 96. K+ and Na+ respectively occupy the clefts of the two discrete polyanions.