Some properties of aqueous solutions of α-NiSO4 · 6H2O

The concentration dependences of the properties of solutions of ??-NiSO₄ · 6H₂O (mineral retgersite) in H₂O and 20% H₂SO₄ have been measured in a wide range of concentrations (up to ??20 solvent molecules per dissolved-salt molecule). It is shown that the solution density, the light absorption coefficient at a wavelength of 394 nm, and the intensity of the Raman scattering peak characteristic of the sulfate ion depend linearly on the bulk salt concentration in the solutions. No shift of the Raman peak as a result of a change in the concentration was observed. These facts indicate that the type of dissolved particles and the character of interactions between them and with the solvent remain the same with an increase in the salt concentration. The data in the literature on the formation of ion pairs in retgersite solutions are discussed.     

Crystal structure of Zn4Na(OH)6SO4Cl·6H2O

The structure of Zn₄Na(OH)₆SO₄Cl·6H₂O, a secondary mineral from Hettstedt, Germany, was determined by single-crystal X-ray diffraction. The crystals are hexagonal,a=8.413(8),c=13.095(24) Å, space group $P\bar 3$ , Z=2. The structure was refined to R=0.0554 and R_w=0.0903 for 970 reflections with I≥3σ(I). The structure can be described as zinc hydroxide layers perpendicular toc, from which sulfates and chlorides extend. The layers are held together by a system of hydrogen bonds involving hexaaquo Na⁺ ions which occupy the interlayer space.     

Structure of 6β-acetoxyprogesterone,C23H32O4

The X-ray crystal structure of 6-acetoxyprogesterone, C₂₃H₃₂O₄, has been determined. This compound crystallizes in space groupP2₁2₁2₁ witha=13.195(3),b=15.035(4),c=10.705(3) Å,V=2139.8(9) ų,M _r=372.5,Z=4,D _x=1.156g cm^–3; MoK radiation (=0.7107 Å),=0.72 cm^–1,F(000)=808;R=0.069, andR _w=0.052 for 1292 reflections. RingA adopts a normal 1,2-half-chair conformation. The side chain is typical for a 20-ketosteroid conformation.     

Crystal structure of aminoguanidinium hexahydro-closo-hexaborate dihydrate, (CN4H7)2B6H6 · 2H2O

The (HAgu)₂B₆H₆ · 2H₂O compound was synthesized and its crystal structure was determined [R = 0.0385 for 2018 reflections with I > 2σ(I)]. The structure consists of HAgu ⁺ cations, centrosymmetric B₆H ₆ ^2? anions, and water molecules. The anions have an almost regular octahedral structure. The bond lengths and angles lie within the following narrow ranges: B-B, 1.715–1.726(2) Å; B-H, 1.08–1.14(2) Å; B-B-B, 59.72°–60.29(9)° and 89.63°–90.20(11)°; and B-B-H, 133.2°–137.0(9)°. The HAgu ⁺ cations and water molecules are involved in the O-H?O, N-H?O, and N-N?N hydrogen bonds and participate in numerous (N, O)-H?H-B specific interactions with the B₆H ₆ ^2? anions, which results in splitting and high-frequency shift of the band of B-H stretching vibrations in the IR spectrum.     

Interferometric study of the growth kinetics of K2Co(SO4)2 · 6H2O and K2Ni(SO4)2 · 6H2O crystals

Crystallography Reports - The growth kinetics of the (001) and (110) faces of K2Co(SO4)2 · 6H2O and K2Ni(SO4)2 · 6H2O crystals in the kinetic mode has been in situ investigated for the...     

Structure of 6α-methyl-17α-hydroxyprogesterone butanoate,C26H38O4

The title compound crystallizes in space groupP2₁2₁2₁ with lattice constantsa=16.253(3),b=17.107(3), andc=8.486(2) Å. The A ring has 1,2-half-chair conformation. The calculated steric energy of a 6-methyl-17-ester progesterone molecule is lower by about 4 kJ/mol for the normal A-ring conformation. The progesterone side chain has typical conformation for 17-ester steroids; the C(16)-C(17)-C(20)-O(20) torsion angle is –24.9(4)°.     

Metal-hydroxycarboxylate interactions: syntheses and structures of K2[VO2(C6H6O7)]2·4H2O and (NH4)2[VO2(C6H6O7)]2·2H2O

Potassium and ammonium dimeric (citrato)dioxovanadium(V) hydrate K₂[VO₂(H₂cit)]₂·4H₂O1 and (NH₄)₂[VO₂(H₂cit)]₂·2H₂O2 (H₄cit=citric acid) have been prepared and characterized by X-ray structure analyses. Vanadate1 crystallizes in the monoclinic space groupP2₁/n (No. 14) with unit cell parameters:a=9.304(2),b=11.756(2),c=11.911(2)Å, =111.72(3)°, andD _c=1.911 g/cm³,Z=2; Vanadate2 also crystallizes in the monoclinic space groupP2₁/n with unit cell parameters:a=9.719(2),b=11.111(3),c=11.294(2)Å, =109.03(2)°, andD _c=1.781 g/cm³,Z=2. Each dimer contains a centro-symmetric planar four-member V₂O₂ ring with two exocyclic citrate entities coordinated by the oxygen atoms of the hydroxy-and -carboxylate ligands, while the other two -carboxylate groups remain uncomplexed. Principal dimensions of the V–O bonds are 1.986(4)_av (hydroxy) and 1.980(3)Å(-carboxyl) for vanadate1, 1.988(2)_av (hydroxy) and 1.974(3)Å(-carboxyl) for vanadate2.     

Structure of 6β-hydroxy-4-androsten-3,17-dione monohydrate,C19H27O3·H2O

The structure of the title compound was determined by X-rays:M _r =319.4,P2₁2₁2₁,a=7.753(3),b=10.566(8),c=20.997(10) Å,Z=4 andD _x =1.171 M gm^–3. FinalR=0.042 (R _w =0.041) for 1814 unique reflections. The water molecule is the hydrogen donor to O3 and O17 and an hydrogen acceptor from the O17 hydroxyl group.     

Crystal structure of a new mineral lahnsteinite Zn4(SO4)(OH)6 · 3H2O

A sample of a new mineral from the oxidation zone of the hydrothermal Pb, Zn, Ag Friedrichssegen deposit (Rhineland-Palatinate, Germany) was studied by single-crystal X-ray diffraction. The parameters of the triclinic (pseudoorthorhombic) unit cell are found to be a = 8.312(1) ?, b = 14.545(1) ?, c = 18.504(2) ?, ?? = 89.71 (1)°, ?? = 90.05(1)°, ?? = 90.13(1)°, and V = 2237.3(3) ?³. The structure is solved by direct methods into the sp. gr. P1 and refined to an R factor of 10.7% using 3788 reflections with |F| > 3??(F) in the isotropic-anisotropic approximation. The crystallochemical formula of lahnsteinite (Z = 8) is [(Zn_2.6Fe_0.3Cu_0.1)^VI(OH)₃][Zn^IV(OH)₃(H₂O)][SO₄] · 2H₂O, where the compositions of the layer composed of Zn octahedra and isolated Zn and S tetrahedra are given in square brackets. The mineral under study is chemically and structurally similar to namuwite and is a natural analog of synthetic zinc hydroxide sulfate trihydrate.     

Crystal structure of N-benzylmethylammonium dihydrogen-monophosphate monohydrate, [C6H5CH2NH2CH3]H2PO4·H2O

The salt N-benzylmethylammonium dihydrogenmonophosphate monohydrate is monoclinic with the following unit cell dimensions: a = 6.356(1)Å, b = 8.385(7)Å, c = 11.472(5)Å, = 104.32(1)°, space group P2₁ with Z = 2. The structure consists of infinite parallel two-dimensional [110] planes built of mutually connected ions and water molecules by strong O–H···O and N–H···O hydrogen bonding. There are no contacts other than normal van der Waals interactions between the layers.     

Crystal structure of radical cation salt (BEDT-TTF)4(GaCl4)2 · C6H5CH3

A new radical cation salt based on bis(ethylenedithio)tetrathiafulvalene (BEDT-TTF) with the tetrahedral anion GaCl ₄ ^? , namely, (BEDT-TTF)₄(GaCl₄)₂ · C₆H₅CH₃, has been synthesized. The crystal structure of this salt is determined by X-ray diffraction analysis [a = 31.757(2) Å, b = 6.8063(3) Å, c = 34.879(2) Å, β = 90.453(4)°, V = 7538.8(7) ų, space group I2/c, and Z = 4]. In the structure, the radical cation layers alternate with the anion layers along the c-axis. The anion layers consist of the GaCl ₄ ^? tetrahedra and solvent molecules. The packing of BEDT-TTF molecules in the radical cation layer differs from that in the structure of the known salt (BEDT-TTF)₂GaCl₄, even though both compounds exhibit semiconductor properties.     

Synthesis and structure of (H2O·HBF4)2(18-crown-6)

The title compound has been prepared by the addition of fluoroboric acid to 18-crown-6 in toluene. The compound crystallizes in the triclinic space group P¯1 witha=7.341(2),b=8.364(2),c=10.631(3)Å,=71.48(2),=67.91(2), =67.94(2)°, andD _c =1.44 g cm^–3 forZ=1. The final conventionalR value was 0.079 based on 1575 observed reflections. The molecule resides on a center of inversion. The (H₂O·HBF₄) moieties are best viewed as fluoroboric acid monohydrate molecules hydrogen bonded to the crown ether, one above and one below the plane of the crown. The FO(water) hydrogen bond separation is 2.474(5)Å, and the O(crown)O(water) separations are 2.834(5) and 2.841(6) Å. The oxygen atoms of the crown ether are planar to 0.23 Å.     

Growth and Study of Properties of Mixed Crystals (NH4)2NixCo1 –x(SO4)2 · 6H2O

Crystallography Reports - Mixed crystals (NH4)2NixCo1 –x(SO4)2 · 6H2O have been grown from aqueous solutions of different compositions by reducing the solution temperature in two growth...     

Crystal and molecular structures of potassium cobalt hydrogen phthalate K2[Co(H2O)6](C8H5O4)4 ⋅ 4H2O and mechanism of Co2+ impurity trapping in KAP crystals

The single-crystal X-ray diffraction analysis of K₂[Co(H₂O)₆](C₈H₅O₄)₄ ? 4H₂O has been carried out. The K₂[Co(H₂O)₆](C₈H₅O₄)₄ ? 4H₂O single crystals are obtained in attempting to grow the KAP crystals with the maximum possible content of Co²⁺ impurity cations. The crystals are isostructural to the earlier-studied similar crystals with Ni(II). The structure is formed by double layers of biphthalate anions and the Co²⁺ and K⁺ cations in between. The Co²⁺ cations are coordinated only by water molecules, whereas the coordination of the K⁺ cations involves both the biphthalate anions and water molecules. A detailed crystal chemical analysis, together with the data on the growth kinetics of KAP crystals in the presence of Co²⁺ and the mass-spectrometric data obtained earlier for the KAP crystals, leads to the conclusion that the Co²⁺ impurity cations should be located in the form of the [Co(H₂O)₆]²⁺ cationic complexes in the interblock layers of the KAP crystals.     

α-NiSO4·6H2O晶体生长与光学性质

用水溶液降温法生长出光学品级的α-NiSO4·6H2O大单晶,对晶体的透过光谱和(001)晶面的X射线衍射性能进行了测试和表征.     

Ni(C6H12N4)2SO4·4H2O晶体的生长、热学和光谱性质

六次甲基四胺(C6H12N4,HMTA)部分取代六水合硫酸镍(NSH)晶体结构中的配位水,合成Ni(C6H12N4)2SO4·4H2O(NSH-HMTA)晶体材料.采用称量法测定了NSH-HMTA晶体的溶解度曲线,应用水溶液降温法在温度区间56 ～44℃之间生长出6 mm×6 mm×2 mm尺寸的晶体,生长速度约为0.5 mm/d.通过等离子发射光谱分析所生长晶体中镍离子含量,X射线单晶衍射用于验证晶体的结构.采用热重法(TGA)和差热分析法(DTA)测定晶体脱水温度和分解温度分别为93℃、1 14℃.测量晶体的紫外-可见光谱特性,其紫外波段透过峰位于波长为307 nm处,比NSH晶体(287 nm)红移了约20 nm,HMTA与Ni2+配位提高了Ni2+的3A2g光谱项的能级,3A2g→3T1g(P)所需能量更低,导致吸收谱红移.     

Synthesis,crystal structure and spectral studies of the complex [Ni(C3H4N2)4(H2O)2]·(C6H4COSO2N)2

The title compound has been synthesized and its crystal structure determined at room temperature.M _r =731.39, triclinic, space groupP¯1,a=9.020(3),b=11.280(7),c=7.784(2)Å,=97.05(4),=97.08(2), =105.32(4)°, U=748(1)ų,Z=1,D _calc.=1.624 g/cm³. The finalR is 0.030 for 3095 independent observed reflections withI3(I). The crystal structure consists of repeated [Ni(im)₄(H₂O)₂]²⁺ cations and noncoordinated saccharin anions. In the complex cation [Ni(im)₄(H₂O)₂]²⁺, Ni² is bonded to four N atoms from four imidazole molecules and two O atoms from two water molecules forming an approximately square octahedral stereochemistry. The d-d transition spectrum of the title compound is also reported and is explained perfectly with the scaling radial theory which was proposed by us.     

Effect of growth conditions on the functional properties of K2Co(SO4)2·6H2O crystals

K₂Co(SO₄)₂ · 6H₂O single crystals of optical quality have been grown and the effect of solution pH on their solubility and transmission spectra has been investigated. A kinetic growth curve is obtained for the (110) face and the onset temperature of dehydration is established for single-crystal samples. The structural quality of single crystals grown at different supersaturations is analyzed.     

Structure of 6-methyl-3,20-dioxo-4,6-pregnadien-17α-yl acetate,C24H32O4

The X-ray structure of 6-methyl-3,20-dioxo-4,6-pregnadien-17-yl acetate is reported. The crystals are monoclinic, space groupP2₁,Z=4,a=28.955(7),b=6.597(2),c=11.064(3) Å,/gb=90.80(2) °. The two crystallographically independent molecules have very similar overall geometries. The A rings have intermediate sofa-half-chair conformations and are bent relative to the steroid skeleton. The conformation of the 17-progesterone side chain is stabilized by the 17-ester substituent; the C(16)-C(17)-C(20)-O(20) torsion angle is –19.4(6) and –20.6(7)°.     

Synthesis and structure determination of a new layered zincophosphate: [H2N2C6H16]0.5[Zn2(PO4)(HPO4)(H2O)]·H2O

The synthesis and crystal structure of a new microporous zincophosphate are described. [H₂N₂C₆H₁₆]_0.5[Zn₂(PO₄)(HPO₄)(H₂O)]·H₂O crystallizes in the triclinic space group P1¯ with a = 8.822(4), b = 9.236(4), c = 8.451(3) Å, = 67.19(3), = 91.32(3), = 111.10(3)°, V = 586.7(4) ų and Z = 2. This new material consists of infinite two-dimensional anionic layers alternated with planes containing organic diprotonated templates, N, N, N, N-tetramethylethylenediamine [H₂N₂C₆H₁₆]²⁺ molecules. The framework structure is built up of ZnO₄, ZnO₃OH₂, PO₄, and PO₃OH tetrahedra, linked through oxygen vertices. The presence of terminal OH₂ and OH groups, leads to an open structure containing four- and eight-rings. The organic molecules are interconnected to the framework through hydrogen bonds.