Crystal growth and structure of KBi(WO4)2 single crystals

Potassium bismuth tungstate [KBi(WO₄)₂] single crystals have been grown by the top‐seeded solution growth technique. Bulk crystal with dimensions up to several centimeters is obtained for the first time. Several self‐flux systems have been used for the growth from the solution and the experiments using K₂W₂O₇ as a solvent are detailed. Powder and single crystal X‐ray diffraction of this crystal are reported. The structure refinement shows that KBi(WO₄)₂ crystallizes in the monoclinic space group C2/c, with a=10.837(3), b=10.586(3), c=7.622(2)Å, β=130.860(3)°, V=661.4(3)ų, and Z=4. (© 2006 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Synthesis and crystal structure of hexakis(N-methylimidazole) iron(II) pyridine-2-sulfonate

The compound [Fe(C₄H₆N₂)₆][C₅H₄NSO₃]₂ crystallized in the monoclinic space group, P2₁/n with unit cell parameters: a = 13.676(3), b = 8.345(2), c = 18.663(4) Å, = 106.40(3)° and Z = 2. The title compound consists of a [Fe(C₄H₆N₂)₆]⁺² hexacoordinated iron(II) cation and two C₅H₄NSO^– ₃ anions. In the cation the iron atom is coordinated to six N-methylimidazole imine nitrogen atoms in a distorted octahedral arrangement. The N1,N5,N1ⁱ,N5ⁱ atoms are coplanar and the iron lies in this plane.     

Crystal structure and molecular stereochemistry of polymeric Cu2(DMP)4(DMSO) as a platform for phosphate diester binding

Treatment of a solution of CuCl₂ in dimethyl phosphate (DMP) in an inert solvent under nitrogen atmosphere resulted in a light blue fluorescence powder. Slow evaporation of H₂O‐DMSO solution of this powder led to the formation of blue‐sky crystals of a new polymeric Cu(II) complex, with a unit cell composed of Cu₂(DMP)₄(DMSO), (1). The crystal and molecular structure of the complex was established crystallographically. Compound (1) crystallizes in the monoclinic space group P2₁/n with a = 12.8920(11)Å, b = 13.1966(11)Å, c = 14.7926(13)Å, α = 90°, β = 98.943(2)°, γ = 90° and Z = 4. A square pyramidal environment for the metal center is established by coordination of oxygen atoms of four bridging DMP ligands in the basal positions and a tri‐centered oxygen atom of DMSO in the apical disposition. The sixth position is also affected by a weak interaction with the sulfur atom of DMSO. The phosphorous atom in the bridging DMP is arranged in a deformed tetrahedron with gg conformation for methyl esters with C_2v symmetry. Accordingly, the angles of methoxy substituents are unexpectedly smaller than the bridging oxygens, and synchronous z‐in and z‐out distortions are suggested for DMP anion. The oxygen atom of SOCuCu’ fragment derived from DMSO, functions as a tri‐centered nuclei lie almost in a trigonal triangle environment. This study helps provide further insights into the binding nature of phosphate esters to the active sites of enzymes, which catalyze phosphoryl transfer reactions. (© 2006 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Crystal structure of (diphenyl)(morpholino)phosphiniminocyclotrithiazene

The title compound (C₆H₅)₂(OC₄H₈N)P=N–S₃N₃ crystallizes in the space group with unit cell parametersa=9.3900(2),b=9.4747(1),c=11.3850(3) Å, =95.73(4), =96.85(6), =104.26(2)^o, and Z=2. The tricoordinated sulfur of the cyclotrithiazene ring deviates from the mean plane of other skeletal atoms by 0.683(4) Å. The angle at this atom is the smallest in the ring and is enclosed by the longest S–N bonds observed in the ring.     

Crystal structure and spectroscopic studies of a new organic monohydrogenmonophosphate dihydrate

The crystal synthesis and structure of a new organic monohydrogenmophosphate (3,4‐Cl₂‐CH₂C₆H₃NH₃)₂HPO₄·2H₂O are reported. This compound crystallizes in the monoclinic P2₁/n with a = 9.081(7) Å, b = 6.501(5) Å, c = 35.423(12) Å, β = 91.09(5)°, V = 2090.9(2) ų, and Z = 4. Crystal structure was solved and refined to R = 0.042, using 2543 independent reflections. It can be described by inorganic layers, including the HPO₄^‐ anions and the H₂O molecules, parallel to (a, b) planes and situated at z = 0 and z = 1/2. The interlayer spacing is occupied by the organic molecules which perform different interactions around the 3D network cohesion. A characterization of this compound by solid‐state (¹³C, ³¹P) MAS NMR and IR spectroscopies is also reported. (© 2007 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Crystal growth and structure determination of the new silicate K3ScSi2O7

Single crystals of the new three-dimensional silicate K₃ScSi₂O₇ were obtained via a high temperature flux method and characterized by single crystal X-ray diffraction. K₃ScSi₂O₇ crystallizes in the space group P6₃/mmc with a = 5.60650(10) Å, c = 13.6420(4) Å. The structure contains sheets of ScO₆ octahedra that are connected via Si₂O₇ bridging groups.     

Crystal structure of bis(2-butyl-4-chloro-imidazole)5-iminoethane

The title compound (C₁₈H₂₆N₆Cl₂) crystallizes in monoclinic space group P2₁/c with a = 14.867(4) Å}, b = 7.758(2) Å}, c = 9.671(3) Å}, = 108.78(1), V = 1056.0(5) Å}³, Z = 2, D_cal = 1.250 Mg/m³ at T = 293 K. The structure was solved by direct methods and refined by full-matrix least-squares procedures to final R = 0.0650 and wR = 0.1719 using 2493 reflections. The imidazole ring is planar and the n-butyl chain adopts an extended conformation. The molecules in the crystal are stabilized by N–H s N type of intermolecular hydrogen bondings in addition to van der Waals forces.     

Crystal structure of 2,2,4,7,7-pentamethyl-3,6-dithiaoctane tetracarbonyl tungsten(0)

The x-ray crystal structure of the complex ²-PDOW(CO)₄ (five-membered ring, PDO = 2, 2, 4, 7, 7-pentamethyl-3,6-dithiaoctane) is reported. The complex crystallizes in the monoclinic crystal system, space group P2₁/c, [#14] with unit cell parameters a = 14.002(14) Å, b = 9.340(10) Å, c = 15.094(12) Å, = 92.67(4)°, V = 1972(3) ų; Z = 4. The arrangement of the ligands around the metal atom is distorted from octahedral geometry. Large C–O bond distances and short W–C bond distances of the carbonyl groups located at a trans position with respect to PDO is indicative of a trans influence. The W–S(1) and W–S(2) bond distances of 2.545(3) and 2.545(2) Å, respectively, are shorter than observed for closely related complexes.     

Crystal and molecular structure of trans-bis(dodecylamine) bis(dimethylglyoximato)cobalt(III) nitrite

An octahedral geometry for the molecule of the title complex with very slight distortions around Co(III) is confirmed by single-crystal X-ray diffraction study. The molecular structure of the complex has been shown to contain two dodecylamine moieties in the trans orientations, two N-bonded dimethylglyoximato (DMG) groups and an uncoordinated nitrite ion.     

Crystal structure of phenyl-substituted cyclopentenes

The crystal structures of two stereoisomers of tetraphenyl- and pentaphenyl-substituted cyclopentenes 1 and 2 have been determined by X-ray analysis. An envelope conformation ¹E has been ascertained for the cis isomer 1a, whereas the cis, cis isomer 2a, which crystallizes in two different space groups, P1¯ and P2₁/n, displays a twisted ²T₁ conformation. The phenyl substituents are all tilted with respect to the cyclopentene ring in both structures. Compound 1a crystallizes in the space group P2₁/a with a = 18.553(3), b = 6.006(2), c = 19.355(5), = 102.67(4)°, and V = 2104.2(g) ų for Z = 4; compound 2a ^I crystallizes in P2₁/n with a = 10.064(2), b = 20.756(5), c = 12.245(3) Å, = 95.21(2)°, and V = 2547(1) ų for Z = 4; compound 2aII crystallizes in P1¯ with a = 10.117(3), b = 11.750(2), c = 12.359(2) Å, = 111.25(2), = 94.84(2), = 108.78(2)°, and V = 1262.3(6) ų for Z = 2.     

Crystal structure of dicalcium potassium trihydrogen bis(pyrophosphate) trihydrate

The crystal structure of Ca₂KH₃(P₂O₇)₂·3H₂O has been determined by single crystal X-ray diffraction. Crystals are monoclinic, space groupP2₁/n witha=10.518(3),b=19.253(9),c=7.340(3)Å,=90.07(2)°, andZ=4. The structure was refined toR=0.048 andR _w=0.044 for 1839 reflections withI3(I). The structure consists of a compact assembly of Ca, K, HP₂O₇, and H₂P₂O₇ ions and three water molecules arranged in layers perpendicular to theb-axis. The two independent Ca ions and the HP₂O₇ ion comprise one layer; K and H₂P₂O₇ ions and the three water molecules form an interstitial layer. Coordinations of the two independent Ca ions are quite similar, but the environments of HP₂O₇ and H₂P₂O₇ ions are quite different, probably due to their locations in different layers. The general structural features are quite similar to those of Ca(NH₄)HP₂O₇.Certain commercial materials and equipments are identified in this paper to specify the experimental procedure. In no instance does such identification imply recommendation or endorsement by the National Institute of Standards and Technology or the ADA Health Foundation or that the material or equipment identified is necessarily the best available for the purpose.     

Crystal structure and EPR spectra of glycilglycilglycinocopper(II)bromide sesquihydrate

The title compound, Cu(glyglygly)Br·1·5H₂O, crystallizes in the space group C2/c, with a = 21.468(7), b = 6.716(5), c = 16.166(6) Å, = 98.39°, and Z = 8. The tripeptide is bonded to one Cu(II) ion through the nitrogen [Cu–N=1.97(1)Å] and oxygen [Cu–O=2.019(8)Å] atoms of the amino end glycine residue and to another Cu(II) through one oxygen atom [Cu–O=1.931(9)Å] of the terminal carboxyl group. This give rise to covalently bonded and infinite ···–Cu–tripeptide–Cu–··· chains. These chains are linked to one another by a network of H-bonds involving the water molecules and bromide ions. The Cu(II) ion is in a distorted tetragonal pyramidal coordination polyhedron. At the corner of the base of the pyramid are the terminal glycine nitrogen and oxygen atoms of one tripeptide, a carboxylic oxygen of another tripeptide and a bromide ion. The fivefold coordination is completed with a water molecule at the top of the pyramid [Cu–Ow=2.286(9)Å]. For all orientations of the applied magnetic field the single crystal EPR spectra display a single anisotropic exchange collapsed resonance without hyperfine structure. Its position was measured in three perpendicular planes and the crystal g-tensor evaluated from the data. This tensor is interpreted in terms of the contributing Cu(II) complexes in the unit cell to deduce the principal values g₁ = 2.273, g₂ = 2.050 and g₃ = 2.131 for the molecular gyromagnetic tensor. We also discuss the magnitude of the exchange interaction between neighboring copper ions in the lattice on the basis of the features in the EPR spectra and the structural information.     

Crystal structure of trismorpholino phosphiniminocyclotrithiazene

The title compound (OC₄H₈N)₃P=N–S₃N₃ crystallizes in a monoclinic crystal system with unit cell parameters a = 8.9996(3), b = 17.2895(7), and c = 12.3648(9) Å, = 90.63(5)°, Z = 4, and space group P2₁/n. Strikingly the exocylic S1–N4 bond length is 1.545(3) ÅR and is accompanied by the largest angle at P–N4–S1 as 131.2(2)°. The tricoordinated sulfur atom of the cyclotrithiazene ring deviates from the mean plane of other five atoms by 0.654(1) Å.     

Crystal and molecular structure of 6,7-benzo-3,4 (1,4-dimethoxy-2,3-naphtho)-1,5-dioxosuberane

The crystal and molecular structure of the title compound (2) C₂₁H₁₆O₄ has been determined by an X-ray analysis, by direct methods from diffractometer data and refined by full-matrix least squares. The compound (2) crystallizes in the space group P2₁/a, with cell parameters:a=36.432(5),b=5.512(3),c=8.269(5) Å, =108.0(3)°,z=4,D _c =1.397 g/cm^–3,R=7.8 for 1136 observed reflections. The conformation of the tetracyclic ring system shows a folding of two planar parts of the carbon skeleton about an axis passing thorough C8 and C16 of the seven membered ring C.     

Crystal structure of a novel tertiary phosphine coordination complex: dichlorobis(tribenzylphosphine)nickel(II)

The title compound dichlorobis(tribenzylphosphine)nickel(II), Ni[P(CH₂C₆H₅)₃]₂Cl₂, belongs to a type of tertiary phosphine coordination complex, M(PR₃)₂X₂. There are two molecules in the unit cell which do not appear to interact chemically. Both molecules have a trans-square planar configuration with each nickel atom on a center of symmetry. Three benzyl groups are bonded to each phosphorus atom as rotors in a propeller, and the threefold axis is along the P—Ni bond, which has a mean length of 2.23(1) Å. Crystal data: C₄₂H₄₂Cl₂NiP₂, Triclinic, space group , a = 10.4892(15) b = 10.5249(12) c = 19.453(2) Å, = 83.872(8), = 76.839(9), = 62.241(8)°, V = 1850.5(4) ų, Z = 2. There is an intramolecular hydrogen bond between the C3 and C11 atoms.     

水热法KTP晶体生长与宏观缺陷研究

本文报道了水热法KTP晶体的生长工艺及晶体生长形态,系统研究了水热法KTP晶体的宏观缺陷,其宏观缺陷主要为添晶、生长脊线、裂隙和包裹体.提出了晶体生长工艺的改进措施,如提高原材料和试剂的纯度、调整籽晶的悬挂方式、减少籽晶的尺寸等,都可以减少晶体的宏观缺陷,提高晶体的质量.//(011)切向的籽晶生长的晶体质量较高,且能很好地应用于激光器件中.     

Formation and structure of ionic (Na, Zn) sulfophosphate glasses

Supercooled ortho- and pyrophosphate melts of the type P₂O₅-EO-A₂O (E = {Zn²⁺, Ca²⁺, Sr²⁺, Ba²⁺, Mg²⁺, Mn²⁺}; A = {Li⁺, Na⁺, K⁺}) exhibit unusually high sulfate solubility. This enables facile fabrication of low-melting sulfophosphate glasses with SO₃ content of up to 25 mol.%. Sulfur is incorporated into those glasses practically exclusively in the form of isolated SO₄^2- groups. The Q-group distribution of phosphate species is dominated by Q¹ and Q⁰ groups, whereby replacing P₂O₅ with SO₃ results in increasing depolymerization. In this way, the glass forming region can readily be extended to compounds with an average number of bridging oxygen per phosphate anion of less than 0.5. In ionic (Na, Zn) sulfophosphate glasses, cations Zn²⁺ and Na²⁺ appear to cluster distinctively around PO₄^3- and SO₄^2- groups, respectively.     

Crystal structure of nimbin

The crystal structure of nimbin has been determined. The crystals are orthorhombic, space groupP2₁2₁2₁ witha=6.790(2),b=14.875(4),c=27.160(8) Å andZ=4. The packing of the molecules in the lattice is due to C?H…O type of hydrogen bonds.     

Crystal structure oftrans-carbonylchlorobis-(tricyclohexylphosphine)iridium(I),trans-Ir(CO)Cl-[P(cyclo-C6H11)3]2, a disordered species

The title compound crystallizes in the centrosymmetric triclinic space group (C ₁ ^l ; No.2) witha=9.9143(10) Å,b=10.2616(11) Å,c=10.7715(10) Å, =113.887(8)°, =109.197(8)°, =90.699(9)°,V=932.78(17) ų andZ=1. A total of 4869 data were collected and merged to a set of 2450 independent reflections; the structure was solved and refined toR=1.42% andwR=1.94%. The molecule lies on a site of symmetry and is disordered, with obvious scrambling of carbonyl and chloride ligands. Resulting bond lengths include Ir–P=2.339(1) Å, Ir–Cl=2.398(4) Å and Ir–CO=1.808(15) Å.     

Crystal structure of a novel bis(guanidiniums) compound incorporated by sulfate anion

Crystal structure of a novel bis(guanidiniums) compound 1 by sulfate anion and water, C₁₁H₂₀N₆OSO₄H₂O, was measured by X-ray crystallographic analysis with an imaging plate method. It possesses space group P2₁/c, with a = 7.6433(15), b = 19.447(4), c = 12.115(2) Å, = 107.81(3)°, and _calc = 1.420 mg/m³ for Z = 4. Crystal data indicate that the architecture network is formed through hydrogen bonds, electrostatic interactions, and arene–arene stacking interaction among the bis(guanidiniums) compound, the sulfate anion and water molecule.