Crystal structure of anhydrous bismuth iodate, Bi(IO3)3

Bismuth iodate was synthesized by precipitation from bismuth nitrate and iodic acid. The powder was dissolved in dilute nitric acid and single crystals were obtained by slow evaporation at 70°C. Bi(IO₃)₃ crystallizes in the monoclinic system, space group P2₁/n (N° 14), a = 8.8882(2) Å, b = 5.9445(2) Å, c = 15.2445(5) Å, = 97.064(1) Å. BiO9 polyhedra are edge-connected forming chains parallel to the b axis; these chains are linked through (IO₃) groups forming layers parallel to (101). The 3D framework is designed by linking these layers through long I–O bonds. DSC analysis shows a remarkable thermal stability.     

Synthesis and Crystal Structure of a New Iodate (Pb0.6Ba0.4)(Pb0.4Ba0.6)[IO3]4 Analogous to Sr[IO3]2

Crystallography Reports - Crystals of a new triclinic iodate with the formula (Pb0.6Ba0.4)(Pb0.4Ba0.6)[IO3]4 (sp. gr. P$$\bar {1}$$) were prepared by hydrothermal synthesis. These crystals are...     

Synthesis and crystal structure of new carbonate NaPb2(CO3)2(OH)

Crystals of a new lead carbonate, NaPb₂(CO₃)₂(OH), sp. gr. P31c, were prepared by hydrothermal synthesis. The crystal structure was established by the heavy-atom method without knowing the exact chemical formula of the compound. The polar structure of the carbonate and the distortion of the pseudosymmetry described by the supergroup P $\bar 3$ 1c are caused by the acentric arrangement of the oxygen atoms providing the satisfactory coordination of Pb and Na atoms. The bonds between a hydroxyl group and two crystallographically independent Pb atoms are directed along the c-axis and have different lengths. The study of the carbonate by the second harmonic generation method in a temperature range of 20–250°C revealed the nonlinear optical properties comparable with the similar properties of quartz. The comparison of the structure of the new carbonate with a number of carbonates demonstrated that the new compound is structurally similar to ewaldite BaCa(CO₃)₂, diorthosilicate NaBa₃[Si₂O₇](OH), and Ba[AlSiO₄]₂ containing a double silicon—oxygen layer.     

Synthesis and crystal structure of Bi(mpo)3 (Hmpo = 2-mercaptopyridine N-oxide)

The synthesis as well as crystal and molecular structure of [Bi(C₅H₄NOS)₃] are reported. The complex crystallizes in the monoclinic system, space group P2₁/n with lattice parameters a = 9.6521(3) Å, b = 10.0659(4) Å, c = 18.4484(7) Å, = 102.13(6)°, and D _calc = 2.227 Mg · m^–3 for Z = 4. It is clear from the packing diagram that the title compound is a dimer via the secondary coordination. Surrounding Bi atom, three five-membered ring planes (Bi,O,N,C,S) make a dihedral angle of 55.91, 54.72, and 26.13° respectively. The whole crystal presents a three-dimensional network structure as each molecule produces four weak C–H O hydrogen bonds and a weak C–H S hydrogen bond.     

Synthesis and crystal structure of Pr(mpo)3(DMSO)2 (Hmpo = 2-mercaptopyridine N-oxide)

A novel rare earth metal complex of 2-mercaptopyridine N-oxide (Hmpo) was synthesized and characterized by single crystal X-ray diffraction, element analysis, and IR spectroscopy. The complex Pr(mpo)₃(DMSO)₂ (Hmpo = 2-mercaptopyridine N-oxide) (DMSO = dimethyl sulfoxide) (C₁₉H₂₄N₃O₅S₅Pr) crystallizes in the triclinic system, space group with lattice parameters a = 9.570(2), b = 9.902(2), c = 15.743(3) Å. = 89.00(3), = 85.54(3), = 62.97(3)°, D _c =1.694 gcm^–3, Mr = 675.62, Z = 2. The coordination number of praseodymium (III) is eight, and its coordination geometry is a somewhat distorted bicapped trigonal prism. Surrounding Pr atom, three five-membered ring planes (Py, O, N, C, S) make dihedral angle of 84.86(7), 75.10(6), and 11.06(9)° respectively. One DMSO molecule is disordered and situated along a twofold axis with half-occupancy (occupation factor, G=0.5).     

Synthesis and crystal structure of [Nd(H2O)2]2(C2O4)3

Some crystals of [Nd(H₂O)₂]₂(C₂O₄)₃ were synthesized hydrothermally by heating at 200°C for 8 days an aqueous suspension of neodymium oxalate decahydrate in presence of terephthallic acid and guanidinium carbonate. They crystallize in the orthorhombic system, space group P2₁2₁2₁, with a = 8.6702(7) Å, b = 9.558(2) Å, and c = 17.009(2) Å. The structure of this complex is built up by two independent neodymium atoms, three bischelating oxalate ligands, and four water molecules forming a rectangle building unit of 6-membered ring, [Ln(H₂O)₂(C₂O₄)]₆. The packing of these units leads to a layer parallel to the plane (001). However, the neodymium atoms of two neighbor layers share an edge of oxalato oxygen atoms thus giving a double-layer. The three dimensionality between these double-layers is insured by hydrogen bonds of water molecules which are bound to the neodymium atoms. There is no zeolitic water molecule. The two neodymium atoms are nine-coordinated. In both cases, the coordination polyhedron can be described as a distorted tricapped trigonal prism.     

Synthesis and crystal structure of bis(2-methylbenzimidazolium) tetrahalocuprate(II)

The crystal structures of 2-methylbenzimidazolium tetrahalocuprates (H2-mebz)₂[CuX₄] (X = Cl and Br) have been detemined. The chloride salt is monoclinic, P2₁/c, with a = 8.540(2) Å, b = 16.591(2) Å, c = 14.303(3) Å, and = 98.69(2)°. The bromide salt is also monoclinic, P2₁/c, with a = 8.316(3) Å, b = 17.436(3) Å, c = 14.747(3) Å, and = 98.82(3)°. Both the compounds contain discrete distorted tetrahedral CuX₄ ^2– anions and almost planar 2-methylbenzimidazolium cations. In the chloride salt, three chloride ions are involved in hydrogen bonding instead of two bromide ions in the bromide salt.     

Synthesis and crystal structure of Na1.28Ni0.86Fe2(PO4)3

A new monophosphate Na_1.28Ni_0.86Fe₂(PO₄)₃ has been synthesized by a flux method and structurally characterized by single-crystal X-ray diffraction. The compound crystallizes in the orthorhombic space group Ibmm with the parameters: a = 6.438(2) Å, b = 10.515(3) Å, c = 13.166(3) Å, Z = 4. The structure is built up from Fe₂O₁₀ units of edge-sharing FeO₆ octahedra, which are connected through the corners of MO₆ (M = Ni²⁺ or a vacancy) octahedra and PO₄ tetrahedra to form a three-dimensional framework analogous to that of -CrPO₄. Of the two crystallographically distinct Na⁺ sites contained in this structure, one is totally filled whereas the other is 28% occupied.     

BiOIO3和Bi2(IO4)(IO3)3晶体电子结构和光学性质研究

采用基于密度泛函理论(DFT)的第一性原理方法对BiOIO3和Bi2(IO4)(IO3)3两种碘酸铋非线性光学晶体的电子结构及光学性质-折射率及双折射率进行了计算研究.结果表明:采用GGA-PBE计算两者的禁带宽度分别为2.385 eV和2.930 eV;选用optados计算BiOIO3和Bi2(IO4)(IO3)3化合物的折射率和双折射率,计算结果表明二者皆具有较大的双折射率.     

Synthesis and crystal structure of bis[N-(2-fluoro-3-methoxy)-salicylideneaminato]copper(II)

The title compound, bis[N-(2-fluoro-3-methoxy)-salicylideneaminato]copper(II) [Cu(C₁₄H₁₂O₂FN)₂] was synthesized and its crystal structure was determined. The title compound is triclinic, space group P with a = 8.552(1), b = 9.645(1), c = 7.871(1) Å, = 108.708(1), = 93.769(1), = 79.429(1), V = 1208.98(1) ų, Z = 2, D _c = 1.696 gcm_–3, (Mo K) = 1.815 mm^–1, R = 0.0369 for 2963 reflections [I>2(I)]. The title compound has crystallographic inversion symmetry with two bidentate Schiff base ligand coordinated to the Cu atom in a square-planar arrangement. The Cu–N1 and Cu–O2 distances are 1.995(1) and 1.885(1) Å, respectively.     

Synthesis and crystal structure of 1-acetyl-3-bromo-3-phenylazetidine and 1-phenyl-2-(N-acetyl-N-formyl)-aminoethanone

1-Acetyl-3-bromo-3-phenylazetidine (1), C₁₁H₁₂BrNO, has been synthesized and characterized by spectroscopic methods and single crystal X-ray analysis. It crystallizes in the space group P2 ₁/c with a = 8.633(1), b = 7.461(1), c = 17.204(1) Å, = 98.403(7)°, V = 1096.2(2) ų, Z = 4, D _calc = 1.540 g cm^–3. The azetidine ring is nearly planar since the four atoms are within ±0.039(5) Å of the mean square plane calculated for the heterocycle. The attempt to obtain a highly strained 2-azetine derivative from the above compound gave, surprisingly, 1-phenyl-2-(N-acetyl-N-formyl)-aminoethanone (2), C₁₁H₁₁NO₃. This compound has been also characterized by spectroscopic methods and single crystal X-ray analysis. It crystallizes in the space group P2₁2₁2₁, with a = 5.4719(3), b = 8.3205(6), c = 23.298(3) Å, V = 1060.7(2) ų, Z = 4, D _calc = 1.286 g cm^–3. The aminoethanone residue is in a near planar conformation where the torsion angles are 7(2)° for N–C–C–=O and –173(2)° for N–C–C–C(Ph).     

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.     

Synthesis and crystal structure of charge-transfer salt (BEDT-TTF) [Pt(mnt)2]

The synthesis and crystal structure of the title organic charge-transfer salt (BEDT-TTF)[Pt(mnt)₂] (BEDT-TTF = bis(ethylenedithio)tetrathiafulvalene; mnt = cis-3,4-dimercapto-2-butenedinitrile) is described. The salt crystallizes in the P1 space group with a = 6.728(2) Å, b = 7.371(2) Å, c = 13.596(4) Å, = 97.904(5)°, = 90.114(5)°, and =108.147(5)°. The stoichiometry between BEDT-TTF and [Pt(mnt)₂] is 1:1. The bond length of the central C=C bond in a BEDT-TTF ion is 1.398 (16) Å, indicating an oxidation state of +1 in BEDT-TTF ion. The structure consists of layers of BEDT-TTF and Pt(mnt)₂ along the c axis. Within each layer, both BEDT-TTF and Pt(mnt)₂ ions form segregated stacks. The stacking is not in a face-to-face manner, but instead, is through a side-by-side arrangement along the a axis, with closest SS contacts of 3.461(3) Å between neighboring BEDT-TTF ions. The structure is consistent with the semiconducting behavior found in the solid.     

Synthesis and the crystal and molecular structure of two modifications of bis(1,10-phenanthroline)trinitratoerbium(III) Er(NO3)3(Phen)2

Two crystalline modifications (I and II) of the phenanthroline complex of erbium nitrate with the same chemical composition, Er(NO₃)₃(Phen)₂, are synthesized by a procedure similar to that used for preparing the phenanthroline complexes of europium nitrate. The crystal structures of these modifications are determined using X-ray diffraction. Crystals of compound I belong to the isostructural family Ln(NO₃)₃(Phen)₂ (Ln = La-Lu). Crystals of compound II are isostructural to those of modification II (new phase) of the Eu(NO₃)₃(Phen)₂ compound. Crystals of I and II are monoclinic, space group C2/c, and Z = 4. The unit cell parameters are as follows: a = 11.126 Å, b = 17.815 Å, c = 12.976 Å, β = 100.45°, and V = 2529 ų for modification I and a = 9.459 Å, b = 15.463 Å, c = 17.076 Å, β = 93.52°, and V = 2493 ų for modification II. The molecular complexes in the structures of compounds I and II are nearly identical. The mean lengths of the Er-N and Er-O bonds are equal to 2.500 and 2.466 Å in compound I and 2.508 and 2.457 Å in compound II, respectively. The difference between the structures of compounds I and II is associated with the difference between intermolecular interactions in the unit cell.     

Synthesis and crystal structure of bis(benzimidazolium) tetrahalocobaltate(II)

The crystal structures of benzimidazolium tetrahalocobaltates (HBz)₂[CoX₄] (X = Cl and Br) have been determined. The chloride salt is triclinic, P-1, with a = 7.670(3) Å, b = 8.307(3) Å, c = 15.730(2) Å, and = 87.37(3)°, = 84.99(3)°, = 67.72(2)°. The bromide salt is monoclinic, C2/c, with a = 15.568(2) Å, b = 8.063(3) Å, c = 5.762(2) Å and = 91.36(3)°. The structures of the two salts are closely related. Both the compounds contain isolated tetrahedral CoX₄ ^2– anions and benzimidazolium cations. In the chloride salt, three chloride ions are involved in strong hydrogen bonding while only two bromide ions participate in the bromide salt. The greater deviation from the ideal tetrahedral geometry in CoBr₄ ^2– can be related to the less extensive hydrogen-bonding network compared to the chloro complex.     

Synthesis and X-ray crystal structure studies of 1-ethyl-3-(2-chlorophenyl)-1,2,3-triazolium perchlorate

The isolation of stable carbenes of the Arduengo (1a) and Wanzlick (2a) type has prompted us to look for stable nitrenium ions of the related structural type 1-ethyl-3-(2-chloropenyl)-1,2,3-triazolium perchlorate (6⁺ClO₄ ^–). The title compound was synthesized and the structure was investigated by X-ray crystallography. It crystallizes in the monoclinic space group P2 ₁/n with cell parameters a = 7.066(4) Å, b = 27.680(6) Å, c = 7.486(2) Å, = 111.22(3)°, and Z = 4. The structure exhibits arrangement of the molecules with intermolecular hydrogen bonds within the layers.     

Trimethylamine-N-oxide induced disproportionation of Re2(CO)10: Synthesis and X-ray crystal structure of [fac-Re(CO)3(ONMe3)3] [ReO4]

An attempted synthesis of [Re(CO₃) (-OH)]₄,1, by reacting Re₂(CO)₁₀ with an excess of NMe₃O in THF resulted instead in isolation of a disproportionation product, [fac-Re(CO)₃(ONMe₃)₃][ReO₄],2. The structure of2 was determined via X-ray crystallography: tri-clinic,P1^¯,a=9.499(5),b=9.841(2),c=13.448(2)Å,=109.92(2),=106.89(3), =93.15(4)°,D _calc=2.22 g^–3 andZ=2. Least-squares refinement based on 1606 observed (I>3(I)) reflections gave final values ofR=0.040 andR _w=0.047. The cation is a distorted octahedron that exhibits several structural manifestations of steric crowding among the bulky NMe₃O ligands.     

Synthesis and crystal structure of bis(3-ammoniumphenyl) sulfone dinitrate [C12H14N2O2S](NO3)2

A new organic nitrate with the formula [C₁₂H₁₄N₂O₂S](NO₃)₂, has been prepared and analyzed by X-ray diffraction. This compound crystallizes in the orthorhombic system: a = 16.771 (3), b = 13.884(2), c = 13.884(2) Å, V = 3232.7(7)ų, Z = 8, space group Pna2₁. Crystal structure can be described as a succession of organic and inorganic layers parallel to b, c plane. H-bonds between the different species play an important role in the three-dimensional network cohesion.