Synthesis and Complexation of 1,2-Bis[(monoaza[15]crown-5)-N-yl]glyoxime. Crystal Structure of (1,2-Bis[(monoaza[15]crown-5)-N-yl]glyoximato)palladium(II)

A new vicinal dioxime ligand with two crown-ether groups, 1,2-bis[(monoaza[15]crown-5)-N-Yl]-glyoxime(LH₂), has been prepared from cyanogen di-N-oxide and monoaza[15]crown-5. Ni(II), Pd(II), and Pt(IV) complexes of LH₂ with or without alkali-metal ions bound to macrocyclic groups have been isolated. The high affinity of [Pd(LH)₂] and [Ni(LH)₂] for the K⁺ ion is observed in solvent extraction experiments. A single-crystal X-ray structure confirms the postulated geometry of [Pd(LH)₂]- The Pd-atom of the centro-symmetric molecule has square-planar PdN₄ coordination where Pd–N distances range from 1.978(3) to 1.970(3) Å. The N–Pd–N intraligand angle is 79.9(1)^°.     

Crystal Structure and ESR Study of a Bimetallic Copper/Iron Crown Ether Inclusion Complex

Bimetallic inclusion complexes have been synthesized by a secondary coordination interaction between the guest complex [Fe(η⁵-C₅H₅)(CO)₂(NH₃)][PF₆] and copper(II) complex 1a or nickel(II) complex lb containing crown-ether hosts. The X-ray crystal-structure analysis established that the Cu,Fe inclusion complex 2 crystallize as a centrosymmetric dimer with a Cu? Cu separation of 3.73 Å and a novel out-of-plane Cu? N interaction. The magnetic parameters for 2 were obtained by ESR and ENDOR spectroscopy. ESR susceptibility measurements down to 6 K exclude the presence of any antiferromagnetic coupling interaction between the Cu^IIcenters of the dimer.     

Crystal Structure and Luminescence of [Eu(TTA)3·DAF]·0.5C7H8 Complex Excited by Visible Light

The non‐ionic europium(III) complex [Eu(TTA)₃·DAF]·0.5C₇H₈ (TTA = 2‐thenoytrifluoroacetonate, DAF = 4, 5‐diazafluoren‐9‐one) was synthesized. The structural determination has been carried out. DAF coordination induces the both excitation spectra in the solid state and solution having a red shift and sensitizes Eu³⁺ luminescence under visible light excitation.     

Crystal Structure of the Menshutkin Complex Benzene · 2SbCl3

Crystals of benzene · 2 SbCl₃, grown from the melt, are triclinic with space group P1 , two formula units per unit cell and lattice constants a = 816.5, b = 821.1,c = 1183.3 pm, α = 94.22, β = 94.00, γ = 108.55° at 295 K. The benzene molecule and the two SbCl₃ molecules are in general positions and form a molecular complex. The distances between the ring plane and the Sb atoms on opposite sides are 330 and 322 pm, similar to the π…Sb interactions in other Menshutkin complexes. Taking into account additional intermolecular contacts of the type Sb…Cl both Sb atoms have a deformed pentagonal-bipyramidal coordination with the benzene molecule in an axial position each. The SbCl₃ molecules form corrugated layers.     

Crystal Structure and Thermal Behaviour of K2[CrF5·H2O]

K₂[CrF₅·H₂O] is monoclinic: a = 9.6835(3) Å, b = 7.7359(2) Å, c = 7.9564(3) Å, β = 95.94(1)°, Z = 4, space group C2/c (n^o 15). Its crystal structure was solved from its X‐ray powder pattern recorded on a powder diffractometer, using for the refinement the Rietveld method. It is built up from isolated octahedral [CrF₅·OH₂]^2? anions separated by potassium cations. The dehydration of K₂[CrF₅·H₂O] leads to anhydrous orthorhombic K₂CrF₅: a = 7.334(2) Å, b = 12.804(4) Å, c = 20.151(5) Å, Z = 16, space group Pbcn (n^o 60), isostructural with K₂FeF₅.     

Crystal Structure of a p-Benzylcalix[5]arene- pyridine Complex

p-Benzylcalix[5]arene.3py (py = pyridine) (1) crystallizes in the triclinic space group P1, a = 10.641(3), b = 13.975(3), c = 24.052(12) Å, = 94.60(4), = 91.51(4), = 111.46(2)°, V = 3312(4) ų, Z = 2. Refinement led to a final conventional R value of 0.065 for 5457 reflections. The calixarene is in a distorted cone conformation. Two pyridine molecules are hydrogen bonded to phenolic oxygen atoms and one of them is included in the hydrophobic cavity of the neighboring calixarene molecule along the a axis.     

Synthesis and Crystal Structure of Mercury(II) Metal Crown Ether with N‐Heterocyclic Carbene Linkage

The mercury(II) metal crown ether ( 2a ) was obtained in high yield by reaction of the carbene precursor 1,2‐bis[N‐(1‐naphthylmethylene)imidazoliumethoxy]benzene dihexafluorophosphate ( 1 ) and Hg(OAc)₂. Addition of NaI to the acetone solution of 2a resulted in precipitation of pale yellow solid 2b . The structures of 2a and 2b were determined by single‐crystal X‐ray diffractometry. Both molecules display a helical conformation with a torsional cycle. The mercury atom in complex 2a is tricoordinated by two intramolecular carbene carbon atoms and an acetate oxygen atom. The mercury atom in complex 2b is tetracoordinated by two intramolecular carbene carbon atoms and two cis‐iodine atoms.     

一个不常见的Ni(Ⅱ)的戊三酮二水杨酰腙配合物的合成和晶体结构

合成了镍的戊三酮二水杨酰腙配合物Ni(C₁₉H₁₆N₄O₅)的两个同质异晶,测定其晶体结构。该配合物的两个晶体均属单斜晶系,空间群为C2/c,晶体1晶胞参数为:a=1.03076(9)nm,b=1.9105(1)nm,c=0.93305(8)nm,β=101.490(4)°,Z=4,μ=1.119mm^-1,R=0.0370;晶体2晶胞参数为:a=2.1949(3)nm,b=0.9901(2)nm,c=0.8568(1)nm,β=92.799(6)°,Z=4,μ=1.084mm^-1,R=0.0440。两个晶体中镍原子由多啮配体的二个酰氧原子和二个肼氮原子形成平面正方形配位。对配合物的红外光谱进行归属。     

New Supramolecular Complex Assembled through Hydrogen Bonds. Crystal Structure of Co(PMBP-tsc)_2 ·2DMF·2H_2O

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Two-dimensional Network Crown Ether Complex. Synthesis and Crystal Structure of 18-Crown-6 Complex: [K(18-C-6)]_2[Cd-(mnt)_2]

ＩｎｔｒｏｄｕｃｔｉｏｎＲｅｃｅｎｔｙｅａｒｓ ,ｃｏｏｒｄｉｎａｔｉｏｎｐｏｌｙｍｅｒｓｈａｖｅｂｅｅｎｒｅ ｃｅｉｖｅｄｍｕｃｈａｔｔｅｎｔｉｏｎｂｅｃａｕｓｅｏｆｔｈｅｉｒｉｎｔｅｒｅｓｔｉｎｇｐｈｙｓｉ ｃａｌｐｒｏｐｅｒｔｉｅｓｓｕｃｈａｓｅｌｅｃｔｒｉｃａｌｃｏｎｄｕｃｔｉｖｉｔｙ ,ｍａｇ ｎｅｔｉｓｍ ,ｎｏｎｌｉｎｅａｒｏｐｔｉｃａｌｐｒｏｐｅｒｔｉｅｓａｎｄｐｏｔｅｎｔｉａｌａｐｐｌｉ ｃａｔｉｏｎｓｉｎｓｅｐａｒａｔｉｏｎａｎｄｃａｔａｌｙｓｔ.1Ｔｈｅｍｏｄｕｌａｒａｐ ｐｒｏａｃｈ…     

Crystal Structure of the Complex of 1,2-Bis[2-(o-hydroxyphenoxy)ethoxy]ethane with Ammonium Thiocyanate

The complex of the podand 1'2-bis[2-(o-hydroxyphenoxy)ethoxy]ethane (L) with ammoniumthiocyanate, [NH₄(SCN)L], was prepared, studied by single crystal X-ray diffraction. This is a host-guestcomplex; in its molecule the podand L is wrapped around the NH ₄ ⁺ cation, which forms hydrogen bondswith all the six oxygen atoms of the podand and one hydrogen bond with the sulfur atom of the SCN^- anion. The geometric parameters (bond lengths, bond angles, torsion angles, etc.) of the molecule of [NH₄(SCN)L] and packing of the molecules in the crystal were determined. The molecules are linked into infinite polymeric chains by intermolecular hydrogen bonds O-H···NCS.