Synthesis and structure of a new molecular octahedral cluster complex Mo<Subscript>6</Subscript>Se<Subscript>8</Subscript>(Ph<Subscript>3</Subscript>P)<Subscript>6</Subscript>·2H<Subscript>2</Subscript>O

Mo₆Se₈(Ph₃P)₆·2H₂O cluster complex has been synthesized and its structure has been defined. The compound is triclinic, space group P1ˉ, with unit cell parameters a = 14.3356(5) Å, b = 15.7882(4) Å, c = 25.3949(8) Å, = 95.9750(10)°, β = 91.1030(10)°, γ= 112.2570(10)°, V = 5279.8(3) ų, Z = 2, ρ_calc = 1.772 g/cm³. The complex has a molecular structure. The molybdenum atoms of the {Mo₆Se₈} cluster nucleus are coordinated by the phosphorus atoms of triphenylphosphine molecules. Original Russian Text Copyright ? 2007 by Yu. V. Mironov, Zh. S. Kozhomuratova, D. Yu. Naumov, and V. E. Fedorov __________ Translated from Zhurnal Strukturnoi Khimii, Vol. 48, No. 2, pp. 389–393, March–April, 2007.     

Palladium clusters Pd<Subscript>4</Subscript>(SR)<Subscript>4</Subscript>(OAc)<Subscript>4</Subscript> and Pd<Subscript>6</Subscript>(SR)<Subscript>12</Subscript> (R = Bu,Ph): Structure and properties

The structures of the Pd₄(SBu)₄(OAc)₄ (I) and Pd₆ (SBu)₁₂ (II) palladium clusters are determined by the X-ray diffraction method. For cluster I: a = 8.650(2), b = 12.314(2), c = 17.659(4) Å, α = 78.03(3)°, β = 86.71(2)°, γ = 78.13(3)°, V = 1800.8(7) ų, ρcalcd = 1.878 g/cm³, space group P \(\bar 1\), Z = 4, N = 3403, R = 0.0468; for structure II: a = 10.748(2), b = 12.840(3), c = 15.233(3) Å, α = 65.31(3)°, β = 70.10(3)°, γ = 72.91(3)°, V = 1767.4(6) ų, ρ calcd = 1.605 g/cm³, space group P \(\bar 1\), Z = 1, N = 3498, R = 0.0729. In cluster I, four Pd atoms form a planar cycle. The neighboring Pd atoms are bound by two acetate or two mercaptide bridges (Pd…Pd 2.95–3.23 Å, Pd…Pd angles 87.15°–92.85°). In cluster II, the Pd atoms form a planar six-membered cycle with Pd···Pd distances of 3.09–3.14 Å, the PdPdPd angles being 118.95°–120.80°. The Pd atoms are linked in pairs by two mercaptide bridges. The formation of clusters I and II in solution is proved by IR spectroscopy and calorimetry. Analogous clusters are formed in solution upon the reaction of palladium(II) diacetate with thiophenol.     

Chromites YbMCr<Subscript>2</Subscript>O<Subscript>5</Subscript> (M = Li,Na, K,Cs): X-ray diffraction study

Ytterbium alkali-metal chromites YbMCr₂O₅ (M = Li, Na, K, Cs) were synthesized by a ceramic procedure from the corresponding oxides and carbonates. Their crystal systems and unit cell parameters were determined by the homology method: for YbLiCr₂O₅, a = 10.34 Å, b = 10.62 Å, c = 15.05 Å, Z = 16, V ^o = 1653.74 ų, ρ_X-ray = 5.85 g/cm³, ρ_pycn = 5.81 ± 0.03 g/cm³; for YbNaCr₂O₅, a = 10.30 Å, b = 10.56 Å, c = 16.46 Å, Z = 16, V ^o = 1790.32 ų, ρ_X-ray = 5.64 g/cm³, ρ_pycn = 5.59 ± 0.07 g/cm³; for YbKCr₂O₅, a = 10.33 Å, b = 10.63 Å, c = 19.93 Å, Z = 16, V ^o = 2188.47 ų, ρ_X-ray = 5.95 g/cm³, ρ_pycn = 5.91 ± 0.03 g/cm³; and for YbCsCr₂O₅, a = 10.34 Å, b = 10.63 Å, c = 18.43 Å, Z = 16, V ^o = 2025.72 ų, ρ_X-ray = 5.19 g/cm³, ρ_pycn = 5.16 ± 0.05 g/cm³.     

Determination of thermal to epithermal neutron flux ratio (f), epithermal neutron flux shape factor (α) and comparator factor (F<Subscript>c</Subscript>) in the Triga Mark II reactor,Malaysia

The thermal to epithermal neutron flux ratio (f or Ø _th /Ø _e ), epithermal neutron flux shape factor (α) and comparator factor (F _c ) are essential parameters when calculating the concentration of sample using k ₀-standardization method in the neutron activation analysis (NAA). The work was performed in the Triga Mark II reactor of Malaysian Institute for Nuclear Technology Research (MINT) using Au/Zr monitor couple. Twenty channels in the reactor have been evaluated and the corresponding thermal to epithermal neutron flux ratios (f) ranged from 11.69 to 47.89. The epithermal neutron flux shape factors (α) were found in the range of ?1.50·10^?1 to 1.59·10^?1 and the comparator factors (F _c ) were calculated within the range of 9.85·10³ to 6.70·10⁴. These results allowed us to study the neutron flux distribution more precisely and established the goodness of fit for k ₀-NAA.     

Synthesis,structure, and antibacterial properties of ternary rare-earth complexes with <Emphasis Type="Italic">o</Emphasis>-methylbenzoic Acid and 1,10-phenanthroline

Ternary rare-earth complexes with o-methylbenzoic acid (o-MBA) and 1,10-phenanthroline (Phen) Ln₂(o-MBA)₆(Phen)₂ · nH₂O(n = 0, 1) (Ln = La, Pr, Y, Yb) were synthesized and characterized by elemental analysis, IR, X-ray diffraction, and TG-DTG means. The complex La₂(o-MBA)₆(Phen)₂ · H₂O (I) is composed of two species of binuclear molecules in which the La³⁺ ion is coordinated with two nitrogen atoms of Phen and seven oxygen atoms of carboxylate groups. The carboxylate groups were bonded to La³⁺ in three modes: chelating-bidentate, bridging-bidentate, and chelating-bridging tridentate. The La³⁺ ion adopted a vigorous distorted monocapped square antiprism geometry. Complex I belongs to the triclinic crystal system, P space group, lattice parameters: a = 13.058(3), b = 12.7584(11), c = 20.773(4) Å, α = 101.18(3)°, β = 93.88(3)°, γ = 115.82(3)°, V = 3283.0(11)ų, Z = 2, ρ_calcd = 1.484 mg/m³, M _r = 1467.06, F(000) = 1476, μ = 1.350 mm^-1. The structure was refined to R _l = 0.0631 and wR ₂ = 0.1504. The antibacterial activity test indicates that these complexes exhibit better antibacterial ability against Escherichia coli and Staphylococcus aureus than the corresponding rare-earth chloride or o-MBA.     

Copper(II) trinuclear complex with trimesic acid salicylidene hydrazone: Synthesis,structure, and magnetic properties

A trinuclear copper(II) complex of trimesic acid salicylidene hydrazone (H₆L) having the composition [Cu₃L · 4Py] · CH₃OH was synthesized and characterized. By X-ray crystallography, the crystals are triclinic: a = 11.7940(4) Å, b = 13.7241(5) Å, c = 15.8993(6) Å, α = 107.4120(10)°, β = 94.2900(10)°, γ = 105.5650(10)°, space group \(P\bar 1\), Z = 2. The number of symmetrically unique reflections having I > 2σ(I) is 7636, R = 0.0465, and R _w = 0.1198. The newly prepared complex contains, in its unit cell, two [Cu₃L · 4Py] molecules which are linked to form a dimer on account of phenoxo bridges (the Cu-O bond length is 2.555 the Cu…Cu distance is 3.348 Separations between them are 9.414, 9.371, and 9.667 of temperature is satisfactorily fitted in terms of a triangular cluster model (?2J = 2.2 cm^?1) with extra intermolecular interactions (zJ′ = 0.4 cm^?1). EPR spectra of solutions at 360–380 K feature a poorly resolved HFS, whose modeling gives a satisfactory result with allowance for the interaction of unpaired electrons with three equivalent copper nuclei (g = 2.098; a _Cu = 25.8 × 10^?4 cm^?1).     

Synthesis and crystal structures of binuclear complexes of cobalt(II) and cadmium(II) diisobutyldithiophosphinates with hexamethylenetetramine

Heteroligand complexes [Co₂(HMTA)(iso-Bu₂PS₂)₄] (I) (μ_eff = 4.67 μB) and [Cd₂(HMTA)(iso-Bu₂PS₂)₄] (II) have been synthesized. Single crystals of compounds I and II have been obtained. The crystals are monoclinic: a = 32.622(2) Å, b = 9.4891(6) Å, c = 21.7570(13) Å, β = 125.774(1)^o, V = 5464.3(6) Å,³, Z = 4, ρ_calcd = 1.331 g/cm³ for I; a = 34.6092(7) Å, b = 9.5595(2) Å, c = 22.3473(5) Å, β = 127.144(1)^o, V = 5893.5(2) Å, Z = 4, ρ_calcd = 1.355 g/cm³ for II; space group for both complexes C2/c. Structures I and II are based on discrete binuclear molecules. The coordination polyhedra of the Co and Cd atoms are distorted tetragonal pyramids NS₄, with the bases formed by four S atoms of two bidentate chelating ligand iso-Bu₂PS ₂ ^? and the axial vertices occupied by N atoms of bidentate bridging HMTA ligand. The character of interaction of the molecules in structures I and II is considered.     

Synthesis and crystal structure of (<Emphasis Type="Italic">o</Emphasis>-Diaminobenzene)<Subscript>2</Subscript> Zn(OAc)<Subscript>2</Subscript>

The treatment of o-diaminobenzene with Zn ( OAc )₂ · 2H₂O in alcohol results in the formation of mononuclear bis(o-diaminobenzene)diacetate Zinc, Zn[C₈H₁₁N₂O₂]₂. Its structure was determined by X-ray diffraction analysis. The complex is also characterized by elemental analysis, ¹H NMR and IR. The crystal is monoclinic space group C2, parameters: a = 16.297(5), b = 4.775(3), c = 11.664(5) Å, β = 97.646(5)°, λ = 1.54184 Å, V = 899.6(7) ų, Z = 2, ρ _c = 1.476 g/cm³, M _r = 399.75, F(000) = 416.0, R ₁ = 0.0594, wR ₂ = 0.1439 for 995 observed reflections with I > 2σ(I).     

Crystal structures of <Emphasis Type="Italic">trans</Emphasis>-[Re<Subscript>6</Subscript>S<Subscript>8</Subscript>(CN)<Subscript>2</Subscript>L<Subscript>4</Subscript>] complexes,L = pyridine or 4-methylpyridine

The structures of three novel octahedral rhenium cluster compounds [Re₆S₈(CN)₂(py)₄]·H₂O (1), [Re₆S₈(CN)₂(4-Mepy)₄] (2), [Re₆S₈(CN)₂(4-Mepy)₄]·4-Mepy (3) (py = pyridine, 4-Mepy = 4-methylpyridine) are determined by X-ray crystallography. Crystal data are: C2/m space group, a = 14.813(1) Å, b = 14.772(1) Å, c = 9.2122(6) Å, β = 119.085(2)°, V = 1761.7(2) ų, d _x = 3.318 g/cm³, R = 0.0585 (1); I4₁/amd space group, a = 16.0018(3) Å, c = 14.7186(5) Å, V = 3768.81(16) ų, d _x = 3.169 g/cm³, R = 0.0489 (2); P2₁/c space group, a = 9.0452(4) Å, b = 15.8065(7) Å, c = 15.2951(6) Å, β = 103.700(2)°, V = 2124.57(16) ų, d _x = 2.957 g/cm³, R = 0.0245 (3). Molecular cluster complexes interact via π-π stacking affording 3D frameworks in 1 and 2 and chains in 3.     

Tetramminenickel hydrogen hexamolybdometalates(III)

Tetramminenickel hydrogen hexamolybdoaluminate and hexamolybdogallate(III) of compositions [Ni(NH₃)₄] · H[AlMo₆O₁₈(OH)₆] · 10H₂O (I) and [Ni(NH₃)₄] · H[GaMo₆O₁₈(OH)₆] · 10H₂O (II) were synthesized and characterized by mass spectrometry, thermogravimetry, X-ray powder diffraction, and IR spectroscopy. Their crystals are triclinic. For compound I, a= 17.30 Å, b= 14.69 Å, c= 10.45 Å, α = 129.07, β = 65.91°, γ = 138.01°, V = 1338.7l ų, ρ_calcd = 2.75g/cm³, Z = 2; for compound II, a = 17.38 Å, b= 14.75 Å, c= 10.51 Å, α = 131.38°, β= 65.96°, γ = 138.09, V = 1338.15 ų, ρ_calcd = 2.68 g/cm³, Z = 2.     

Syntheses,Structures, and Magnetic Properties of Two Mn(II) Coordination Polymers Based on 4-Fluorocinnamic Acid and 1,10-Phenanthroline

Two Mn(II) coordination polymers, {[Mn₃ (Pfca)₆(Phen)₂] · 2DMF} _n (I) and [Mn(Pfca)₂(Phen)(H₂O)] _n (II) (HPfca = 4-fluorocinnamic acid, Phen = 1,10-phenanthroline), were synthesized and characterized by elemental analysis, IR spectroscopy, thermogravimetric analysis, and singlecrystal X-ray diffraction (CIF files CCDC nos. 967513 (I), 1542972 (II)). Complex I crystallizes in the triclinic crystal system, space group Pī with a = 11.0821(11), b = 12.2632(12), c = 15.0288(15) Å, α = 87.3760(10)°, β = 88.4610(10)°, γ = 81.2220(10)°, V = 2016.0(3) Å3, ρ_c = 1.369 g/cm³, M _r = 1662.25, Z = 1, F(000) = 853, μ = 0.543 mm^–1, the final R = 0.0592 and wR = 0.1681 for 15498 observed reflections with I > 2σ(I). Complex II is of monoclinic system, space group P2₁/c with a = 18.0539(19), b = 8.5806(9), c = 18.758(2) Å, β = 116.5700(10)°, V = 2599.0(5) ų, ρ_c = 1.491 g/cm³, M _r = 583.44, Z = 4, F(000) = 1196, μ = 0.567 mm^–1, the final R = 0.0337 and wR = 0.0853 for 18139 observed reflections with I > 2σ(I). Complex I features linear Mn(II)-trinuclear units, which form 1D chain structure through F···F weak interactions, and complex II is 1D polymeric Mn(II)-chains. Antiferromagnetic coupling interactions exist within Mn(II)- carboxylate trinuclear in I (J =–0.40 cm^–1) and Mn(II)-carboxylate chain in II (J =–0.45 cm^–1).     

Synthesis and crystal structure of <Emphasis Type="Italic">N,N</Emphasis>-dimethylbiguanidinium hexafluorosilicate

The complex [(CH₃)₂NC(NH₂)NHC(NH₂)NH₂]SiF₆ (I) was synthesized and its structure was determined by X-ray crystallography. The crystals are monoclinic: a = 7.4346(10) Å, b = 12.7628(10) Å, c = 11.0828(10) Å, β 104.080(10)°, V = 1020.01(18) ų, ρ_calc = 1.780 g/cm³, μ(MoK _α) = 0.302 mm^?1, Z = 4, space group P2₁/c. The crystals of I are composed of SiF ₆ ^2? anions (Si-F, 1.657(2)–1.699(2) Å) and N,N-dimethylbiguanidinium (H₂L²⁺) cations combined in a framework by interionic H-bonds NH···F. In the cations, protonation sites are the terminal imide groups.     

Copper(II) complex with salicylaldehyde <Emphasis Type="Italic">N</Emphasis>-(2-salicylideneiminoglutaryl)hydrazone: Synthesis and structure

A copper(II) complex with salicylaldehyde N-(2-salicylideneiminoglutaryl)hydrazone (H₄L) of the formula [Cu₂L · 2Py]₂ · 8H₂O (I) was obtained and characterized by X-ray diffraction. The crystals are monoclinic, space group P2₁, a = 13.0663 Å, b = 16.5553 Å, c = 17.7650 Å, β = 97.9420°; Z = 4. The complex is tetranuclear with a “dimer-of-dimers” structure in which the copper cations of two binuclear subunits are linked by phenoxy bridges. The EPR spectra of solutions of complex I show a superposition of two signals of four HFS lines (g ₁ = 2.111, a ₁ = 56.8 × 10^?4 cm^?1 and g ₂ = 2.183, a ₂ = 71.0 × 10^?4 cm^?1).     

Crystal structure of potassium dysprosium octacyanotungstate(IV) heptahydrate

The crystal structure of KDyW(CN)₈ · 7H₂O was determined by X-ray diffraction. The crystals are triclinic, space group PI, a = 7.6284(7) Å, b = 9.2435(9) Å, c = 14.4778(14) Å, α = 80.673(11)°, β = 87.561(11)°, γ = 77.603(11)°, V = 983.86(16) ų, Z = 2, ρ_calcd = 2.429 g/cm³, R = 0.0249, w _R = 0.0502 for 3601 independent reflections. The coordination polyhedron of tungsten is a highly deformed tetragonal antiprism [W(CN)₈], that of dysprosium is a tetragonal antiprism [DyN₄(H₂O)₄]. Some cyano groups are bridging being coordinated to tungsten and dysprosium by C and N atoms, respectively, and form a 3D structure via potassium atoms. The coordination polymer can be described as {[K(H₂O)][Dy(H₂O)₄][W(CN)₈]}n· 2nH₂O.     

Syntheses and structures of six-coordinate K[Ga<Superscript>III</Superscript>(Cydta)] · 2H<Subscript>2</Subscript>O and K[Ga<Superscript>III</Superscript>(Pdta)] · 3H<Subscript>2</Subscript>O complexes

The title complexes, K[Ga^III(Cydta)] · 2H₂O(Cydta = trans-1,2-cyclohexanediaminetetraacetic acid) and K[Ga^III(Pdta)] · 3H₂O (Pdta = propylenediaminetetraacetic acid), were prepared, and their structures were studied by IR spectra, elemental analyses, NMR spectra, and single-crystal X-ray diffraction techniques. In the K[Ga^III(Cydta)] · 2H₂O complex, the Ga³⁺ is six-coordinated by the Cydta ligand yielding an octahedral conformation, and the complex crystallizes in the monoclinic system with the P2₁/c space group. The crystal data are as follows: a = 16.5039(19), b = 13.1499(16), c = 8.5204(10) Å, β = 101.650(2)°, V = 1811.0(4) ų, Z = 4, ρ = 1.757 g/cm³, μ = 1.805 mm^?1, F(000) = 984, R = 0.0291, and wR = 0.0698 for 3713 observed reflections with I ≥ 2σ(I). In the K[Ga^III(Pdta)] · 3H₂O complex, the Ga³⁺ is also six-coordinated by the Pdta ligand yielding an almost standard octahedral conformation, and the complex crystallizes in the orthorhombic system with P2₁2₁2₁ space group. The crystal data are as follows: a = 8.8913(10), b = 11.6181(13), c = 17.0227(19) Å, V = 1758.4(3) ų, Z = 4, ρ = 1.757 g/cm³, μ = 1.862 mm^?1, F(000) = 952, R = 0.0288, and wR = 0.0724 for 3556 observed reflections with I ≥ 2σ(I).     

4,7,13,16,21,24-Hexaoxa-1,10-diazoniabicyclo[8.8.8]-hexacosane Bis(nitrate-hydrogennitrate): Synthesis and crystal structure

A crystalline adduct of 2.2.2-cryptand and nitric acid, [H₂(Crypt-222)]²⁺·2(NO ₃ ^? ·HNO₃) (I), is synthesized and studied using X-ray diffraction analysis. The monoclinic structure of compound I (space group C2/c, a = 13.326 Å, b = 15.262 Å, c = 15.020 Å, β = 98.96°, Z = 4) is solved by a direct method and refined by the full-matrix least-squares method in the anisotropic approximation to R = 0.067 for 2647 independent reflections (CAD4 automated diffractometer, λMoK _α radiation). In the structure of compound I, the 2.2.2-cryptand dication lies on an axis 2 and has an endo-endo conformation, for which two H atoms at two protonated N atoms are directed inside the cavity. One of the NO ₃ ^? ·HNO₃ dimers is situated in the inversion center, and the other dimer lies on another axis 2 and is disordered over three orientations. All H atoms in the NO ₃ ^? ·HNO₃ dimers are equiprobably disordered over two close sites. Each of the two NO ₃ ^? ·HNO₃ dimers is formed by the very strong disordered N-O-H···O=N hydrogen bond between the nitric acid molecule and nitrate anion.     

Crystal structures of <Emphasis Type="Italic">trans</Emphasis>-dichlorobis(ethylendiamine) rhodium(III) with univalent anions

The crystal structures of the compounds trans-[Rh(en)₂Cl₂]Cl₂ · H₅O₂ (I), trans-[Rh(en)₂Cl₂]ClO₄ (II), and trans-[Rh(en)₂Cl₂]ReO₄ (III) are determined. The crystal data are: I, a = 10.860(3) Å, b = 7.795(2) Å, c = 9.023(3) Å; β = 111.56(10)°, P2₁/c space group, Z = 4, d _x = 1.875 g/cm³; II, a = 6.593(2) Å, b = 8.309(3) Å, c = 11.922(4) Å, α = 83.55(10)°, β = 79.80(10)°, γ = 75.38(10)°, P \(\bar 1\) space group, Z = 2, d _x = 2.106 g/cm³; III, a = 6.533(2) Å, b = 16.391(4) Å, c = 12.411(3) Å; β = 98.30(10)°, P2₁/c space group, Z = 4, d _x = 2.749 g/cm³. The compounds are examined by IR spectroscopy and powder XRD. The solubility of the isolated crystalline phases in water decreases in the following order: trans-[Rh(en)₂Cl₂]Cl₂·H₅O₂ > trans-[Rh(en)₂Cl₂]ClO₄ > trans-[Rh(en)₂Cl₂]ReO₄.     

Synthesis and structure of novel Mn(II) complex with in situ synthesized ligand

Based on in situ synthesized Schiff base ligand Dppd (Dppd = N-(di(2-pyridyl)methylene)-p-phenylenediamine), a novel dinuclear Mn(II) complex, [Mn₂(Dppd)₄(OAc)₂](ClO₄)₂(CH₂Cl₂)₂ · 2(H₂O) (I), was synthesized and characterized by IR and single-crystal X-ray diffraction. The crystals belong to monoclinic system, space group C2/c with a = 26.3868(2), b = 20.0379(4), c = 19.16260(10)Å, β = 126.6900(10)°, V = 8124.61(18) ų, Z = 4. The complex exhibits a dinuclear structure in which two symmetric Mn(II) atoms adopt somewhat distorted octahedral geometry. The 2D structure is further constructed through intermolecular benzene-benzene offset π···π interactions.     

Synthesis and structure of bis(1,2-diaminoethane) copper(II) bis(<Emphasis Type="Italic">o</Emphasis>-hydroxybenzoate) monohydrate and <Emphasis Type="Italic">trans</Emphasis>-diaquabis(1,2-diaminoethane)copper(II) bis(<Emphasis Type="Italic">o</Emphasis>-aminobenzoate)

X-ray structural analysis has been performed for two complex compounds: Cu(en)₂(o-HB)₂H₂O (I) (a = 16.873(4) Å, b = 8.713(2) Å, c = 14.803(3) Å, β = 91.15(2)°, V = 2175.8(8) ų, C2/c, Z = 4, R(F) = 0.0263, 1516 reflections with I > 3σ (I)) and [Cu(en)₂(OH₂)₂]²⁺(o-AB^?)₂ (II) (a = 7.488(5) Å, b = 22.122(8) Å, c = 7.856(5) Å, β = 118.77(2)°, V = 1140.7(11) ų, P2₁/n, Z = 2, R(F) = 0.0432, 1684 reflections with I > 3σ(I)) synthesized under identical conditions (en is ethylenediamine, o-HB is o-hydroxybenzoate, and o-AB is o-aminobenzoate). Although the compounds were assumed to have similar structures and the Cu-Lig bond lengths and the cis and trans angles are acceptable for an octahedral structure, the geometric parameters of o-HB suggest that the copper atom has a plane square environment.     

Preparation and physicochemical study of sodium hexamolybdometallates(III)

Sodium hexamolybdocobaltate(III) Na₃[CoMo₆O₁₈(OH)₆] · 8H₂O (I) and sodium hexamolybdochromate Na₃[CrMo₆O₁₈(OH)₆] · 8H₂O (II) were synthesized and studied by mass spectrometry, thermogravimetry, powder X-ray diffraction, and IR spectroscopy. The crystals are monoclinic. For compound a = 10.31 Å, b = 10.31 Å, c = 17.55 Å, β = 100.93°, V = 1834.77 ų, ρ_calcd = 3.04 g/cm³, Z = 3; for compound II: a = 10.33 Å, b = 10.33 Å, c = 17.59 Å, β = 100.98°, V = 1835.09 Å3, ρ_calcd = 3.01 g/cm³, Z = 3.