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1.
Absract—Diaqua(2.2.2-Cryptand)strontium dichloride trihydrate [Sr(2.2.2-Crypt)(H2O)2]2+ · 2Cl · 3H2O (I) was prepared and studied by X-ray diffraction. The triclinic structure of I (space group P , a = 9.152 Å, b = 10.140 Å, c = 15.219 Å, = 88.84°, = 88.19°, = 87.62°, Z = 2) was solved by the direct method and refined by full-matrix least-squares calculations in the anisotropic approximation to R = 0.050 for 4188 independent reflections (CAD4 automated diffractometer, CuK radiation). The structure contains the [Sr(2.2.2-Crypt)(H2O)2]2+ host–guest cation. The Sr2+ cation resides in the 2.2.2-cryptand cavity and is coordinated by all eight heteroatoms (6O + 2N) of the cryptand ligand and by two O atoms of water molecules. The Sr2+ coordination polyhedron (C.N. 10) is a highly distorted dibase-centered two-cap trigonal prism. The crystal structure of I contains a branched system of ion–ion (intermolecular) hydrogen bonds O(w)–H···Cl, which connect the complex cations, the Cl anions, and the crystal water molecules to form infinite thick layers parallel to the yz plane.  相似文献   

2.
Twinned and disordered crystals of solvated bis[aqua(2.2.2-cryptand)calcium] hexa(isothiocyanato)calcium 2[Ca(2.2.2-Crypt)(H2O)]2+ · [Ca(NCS)6]4– · Sol (I), where Sol is acetone and/or ethanol and may be water, were synthesized and studied by X-ray diffraction analysis. Structure I (space group P21/n, a = 11.841 Å, b = 21.787 Å, c = 12.377 Å, = 90.90°) was solved by the direct method and refined by the full-matrix least squares method in anisotropic approximation to R = 0.079 from 4168 independent reflections (CAD4 automated diffractometer, MoK ). In crystal form, complex I exists as the two aforesaid complex ions [I1]2+ and [I2]4– in the molar ratio 2 : 1 united through hydrogen bonds. Complex cation I1 is of the guest–host type. Its Ca2+ cation is coordinated by all eight heteroatoms (6O + 2N) of the cryptand ligand and by the O atom of the water molecule; the coordination polyhedron of this Ca2+ cation (CN 9) is irregular. The Ca2+ cation of complex anion I2 (in the crystallographic center of inversion) is coordinated by six N atoms of six neighboring SCN anionic ligands; the coordination polyhedron of this Ca2+ cation (CN 6) is a slightly distorted octahedron.  相似文献   

3.
The aqua complex of podand 1,2-bis(2-(o-hydroxyphenoxy)ethyloxy)ethane (L) with strontium perchlorate of the composition [Sr(ClO4)L(H2O)2]+ · ClO4 · H2O (I) was synthesized and studied using X-ray diffraction analysis: space group P21/c, a = 16.195 Å, b = 11.382 Å, c = 16.646 Å, = 117.01°, Z = 4. The structure was solved by direct method and anisotropically refined by the full-matrix least-squares method to R = 0.069 for 4278 independent reflections (CAD4 autodiffractometer, MoK ). Structure I contains complex cation [Sr(ClO4)L(H2O)2]+ of the host–guest type. The Sr2+ cation (coordination number 9) is coordinated to all six O atoms of the L podand, O atom of a disordered ClO4 ligand, and two O atoms of two water molecules. The coordination polyhedron of Sr2+ is irregular; in a rough approximation, it can be described as a face-centered cube. The crystal structure of I contains an infinite three-dimensional network of the O–H···O hydrogen bonds joining the complex cations, ClO4 anions, and molecules of crystallization water.  相似文献   

4.
The salt tetrakis(isothiocyanato)zinc(II) 4,7,13,16,21,24-hexaoxa-1,10-diazoniabicyclo[8.8.8]hexacosane, [H2(Crypt-222)]2+ · [Zn(NCS)4]2– (I), was synthesized and its structure was determined using X-ray diffraction analysis: space group P21/n, a = 13.734 Å, b = 11.627 Å, c = 20.816 Å, = 91.51°, Z = 4. The structure was solved by direct methods and anisotropically refined by the full-matrix least-squares method to R =0.093 for 4920 independent reflections (CAD4 autodiffractometer, CuK radiation). The structural units of crystal I are 2.2.2-cryptand dications (with two protonated nitrogen atoms) and complex anions [Zn(NCS)4]2–. The coordination polyhedron of the Zn2+ cation is a distorted tetrahedron. The 2.2.2-cryptand dication contains trifurcate N–H(...O)3 hydrogen bonds.  相似文献   

5.
Crystals of bis[(2.2.2-cryptand)sodium] bis[aqua(isothiocyanato)(-isothiocyanato)sodium]: 2[Na(C18H36N2O6)]+ · [Na2(NCS)2(-NCS)2(H2O)2]2– (I) were synthesized and studied by X-ray diffraction analysis. The disordered structure of I (a = 12.715 Å, b = 10.458 Å, c = 21.767 Å, = 102.56°, space group P21/n) was solved by the direct method and refined by the full-matrix least-squares method in anisotropic approximation to R = 0.058 from 3896 independent reflections (CAD4 automated diffractometer, MoK ). The crystal consists of two complex ions [I1]+ and [I2]2– (molar ratio 2 : 1). The Na+ cation of the host–guest cation I1 is coordinated by all eight heteroatoms (6O + 2N) of the cryptand ligand. The coordination polyhedron of this Na+ cation is a distorted cube. The atoms of two groups (CH2–CH2 and CH2–O–CH2–CH2) in the cryptand ligand are disordered over two positions. The independent cation Na+ of the centrosymmetric binuclear complex anion I2 is coordinated by one bifurcated O atom of the disordered water molecule and by three N atoms of the SCN ligands (including two bridging ligands). The coordination polyhedron of this Na+ caiotn is a distorted tetrahedron. The complex ions in the crystal structure of I are united by hydrogen bonds.  相似文献   

6.
Zusammenfassung Die Kristallstruktur von Li2GeO3 wird mit Hilfe dreidimensionalerFourier-Synthesen und nach der Methode der kleinsten Quadrate bestimmt. Li2GeO3 ist isotyp mit Li2SiO3 und enthält [GeO3]2–-Ketten (Zweiereinfachkette). Die Gitterparameter der rhombischen Elementarzelle (C 2v 12 –Cmc21) betragen:a=9,630,b=5,465 undc=4,850 Å. Als mittlere interatomare Abstände wurden erhalten: Ge–O=1,74 und Li–O=2,01 Å.
The crystal structure of Li2GeO3 has been determined by means of 3-dimensional Fourier syntheses and least-squares method. Li2GeO3 is isostructural with Li2SiO3, containing [GeO3]2–-chains (Zweiereinfachkette). The lattice parameters of the orthorhombic cell (C 2v 12 –Cmc21) are:a=9,630;b=5,465 andc=4,850 Å. The average interatomic distances are found to be: Ge–O=1,74 and Li–O=2,01 Å.


Mit 3 Abbildungen  相似文献   

7.
Crystal structures of [Co(MH)2(Thio)2][BF4] · H2O (I) and [Co(DH)2(NH3)2][BF4] (II), where MH is H3C–C(NOH)–C(NO)–H and DH is H3C–C(NOH)–C(NO)–CH3, were determined by X-ray diffraction. The crystals are monoclinic, space group C2/c, unit cell parameters (for I and II, respectively): a = 22.018(2) Å, b = 7.943(1) Å, c = 11.681(1) Å, = 92.68(1)° and a = 21.436(2) Å, b = 6.400(2) Å, c = 12.389(2) Å, = 113.13(1)°. In both cases, the Co(III) coordination polyhedron is a centrosymmetrical trans-octahedron, N4S2 for I and N6 for II. In the crystals of I and II, the complex cations and the outer-sphere [BF4] anions (and the crystal water molecules in I) form elaborate hydrogen bonding system.  相似文献   

8.
Crystalline bis(dibenzo-18-crown-6)rubidium triiodide complex [Rb(DB18C6)2]+ · I3 (I) is synthesized and its structure is studied by X-ray diffraction analysis. The structure of I (space group Pnma, a = 23.854 Å, b = 23.612 Å, c = 7.863 Å, Z = 4) is solved by the direct method and refined by the full-matrix least-squares method in the anisotropic approximation to R = 0.079 against 3990 independent reflections (CAD4 automated diffractometer, MoK ). Structural units of crystal I are the I3 anions and [Rb(DB18C6)2]+ cations. The crystal has the structure intermediate between that of a standard host–guest complex and a sandwich complex. In the structure of complex I, the crystallographic plane with symmetry m passes through the I3 anion (perpendicularly to its axis) and complex cation. The coordination polyhedron of the Rb+ cation is a strongly distorted hexagonal pyramid with the O atom of one crown ligand at the axial vertex and a base of six O atoms of another DB18C6 crown ligand.  相似文献   

9.
The crystal adduct (1 :1) 4,7,13,16,21,24-hexaoxa-1,10-diazoniabicyclo[8.8.8]hexacosane triaquachlorolithium dichloride, [H2(Crypt-222)]2+ · 2Cl · [LiCl(H2O)3] (I), was synthesized and studied using X-ray diffraction analysis. Structure I (space group R3, a = 7.922 Å, c = 37.207 Å, Z = 3) was solved by direct methods and anisotropically refined by the full-matrix least-squares method to R = 0.034 for 1363 independent reflections (CAD4 autodiffractometer, MoK ). Crystal I consists of disordered 2.2.2-cryptand dications, chloride anions, and tetrahedral [LiCl(H2O)3] complexes. All of them lie on threefold axes. There are tridentate +N–H (···O)3 hydrogen bonds in the [H2(Crypt-222)]2+ dication. The crystal structure of adduct I contains a complex interionic hydrogen bonding system.  相似文献   

10.
The crystal structures of complex antimony(III) fluorides RbSbF4 (I) and (C2N4H5)SbF4 (II) were determined. The crystals of I and II are monoclinic; for I: a = 4.628(1) Å, b = 6.167(1) Å, c = 7.922(1) Å, = 100.582(3)°, V = 222.24(7) Å3, Z = 2, (calcd.) = 4.23 g/cm3, (exp.) = 4.25 g/cm3, F(000) = 248, space group P21/m, R = 0.0395; for II: a = 4.678(1) Å, b = 7.339(4) Å, c = 10.185(1) Å, = 90.88(2)°, V = 349.6(2) Å3, Z = 2, (calcd.) = 2.69 g/cm3, (exp.) = 2.70 g/cm3, F(000) = 264, space group P21. The structure of I is formed by Rb+ cations and [SbF4] n n anionic chains composed of SbF5E octahedra with two bridging fluorine atoms. The structure of IIis formed by (C2N4H5)+ cations and isolated [SbF4] anions in which the antimony polyhedra are SbF4E trigonal bipyramids. The relationship between the crystal structures and electrophysical and biological properties of single-charged cation tetrafluoroantimonates(III) was studied.  相似文献   

11.
Crystals of anionic complexes of the composition M[CuCl2(HOCH2CCCH2OH)], where M = NH4 + (I), K+ (II), were isolated from concentrated aqueous solutions of CuCl and MCl (M = NH4 +, K+) in the presence of 2-butyne-1,4-diol. Their structures were studied by X-ray diffraction analysis. Isostructural crystals I and II are orthorhombic; Z = 8, space group Ibam; a = 6.735(1) and 6.666(2) Å, b = 17.206(3) and 16.874(6) Å, c = 15.172(3) and 15.032(4) Å, V = 1758(1) and 1691(1) Å3, respectively. The compounds are built of individual [CuCl2(HOCH2CCCH2OH)] anions; the NH4 + (I) or K+ (II) cations are arranged in the voids between the anions. The -coordinated Cu(I) atoms have trigonal-planar environment of two chlorine atoms and CC bond of the 2-butyne-1,4-diol molecule. The Cu–(CC) distances in the -core are 1.892(4) and 1.887(6) Å, CC are 1.233(5) and 1.228(5) Å in I and II, respectively. In complex I, additional hydrogen bonds Cl···H–NH3 (Cl···H 2.43(4) Å) and O···H–NH3 (O···H 1.97(3) Å) stabilize the structure.  相似文献   

12.
A mixed complex aqua(2.2.2-cryptand)(perchlorato-O)lead(II) diaqua(2.2.2-cryptand)lead(II) tris(perchlorate), [Pb(2.2.2-Crypt)(CIO4)(H2O)]+ [Pb(2.2.2-Crypt)(H2O)2]2+ (ClO 4 ? )3, is synthesized and studied by X-ray diffraction analysis. The crystals are orthorhombic: space group Pbca, a = 19.118 Å, b = 15.360 Å, c = 39.020 Å, Z = 8. The structure is solved by a direct method and refined by the full-matrix least-squares method in the anisotropic approximation to R = 0.089 for 7712 reflections (CAD-4 automated diffractometer, λMoK α radiation). In each of the two complex cations of the host-guest type in the structure, the Pb2+ cation is coordinated by all the eight heteroatoms (6O + 2N) of the cryptand ligand and by two O atoms of the water molecule and ClO 4 ? anion or by two O atoms of two water molecules. In the crystal, alternating complex cations and ClO 4 ? anions are linked into infinite chains (along the z axis) through interionic hydrogen bonds O-H···O-Cl.  相似文献   

13.
The title compound, [La2(H2O)4(C7H3N2O6)6] n (I), synthesized by the hydrothermal reaction of 3,5-dinitrobenzoic acid and 1,10-phenanthroline with La(ClO4)3 · 6H2O crystallizes in the triclinic system, space group P with a = 9.566(2) Å, b = 12.126(3) Å, c = 14.214(3) Å, = 114.614(3)°, = 103.246(3)°, = 97.130(3)°, V = 1413.3(6) Å3, Z = 2, R(F) = 0.0392 and wR(F 2) = 0.0425. In I, each La3+ ion is coordinated by six oxygen atoms of six carboxylate ligands and two oxygen atoms of two coordinated water molecules. The 3,5-dinitrobenzoato anions bridge the La(III) centers to form one-dimensional linear chains, and – interaction between the phenyl rings of 3,5-dinitrobenzoato anions of adjacent linear chains links the chains to engender a two-dimensional network.  相似文献   

14.
X-ray diffraction and spectroscopic data for a new Np(V) compound, namely, [NpO2{OC(NH2)2}5](NO3) (I) are presented. Crystals are monoclinic, space group P21, a = 11.142(2) Å, b = 7.6379(9) Å, c = 11.143(2) Å, = 108.9(1)°, Z = 2, V = 897.1(2) Å3. The neptunium atom has a typical pentagonal-bipyramidal environment with five oxygen atoms of the carbamide molecules in the equatorial plane. The nitrate ion is in the outer sphere. Carbamide is a strong molecular ligand with respect to Np(V) and hence, cation–cation bonds of the NpO2 + ions are not realized in structure I. The wave length of the ff transition in the electronic absorption spectra of crystalline complex I and Np(V) in a saturated carbamide solution is virtually the same and is equal to 991 nm.  相似文献   

15.
Crystals of Ca[CoII(Nta)]2· 6H2O (I), where Nta3–is a nitrilotriacetate ion, were synthesized and studied using X-ray diffraction analysis. They were found to be monoclinic: a= 6.991(1), b= 10.031(1), c= 16.238(3) Å, = 98.50(1)°, V= 1126.2(3) Å3, space group P21/n, Z= 2, R 1= 0.0241, wR 2= 0.0636, GOOF = 1.050 (for 3132 reflections with I> 2(I)). Structure Iis composed of {[Co(Nta)(H2O)]}1anion chains united by Ca2+cations into a three-dimensional framework. The coordination polyhedra of Co and Ca atoms are distorted octahedra. The Co(II) atom environment includes atoms N(1), O(1), O(3), and O(5) of one Nta3–ligand, a carbonyl O(2)" atom of the neighboring anion fragment, and an O(w1) atom of the water molecule. The shortest bond is formed by the Co atom with the bridging O(2)" atom in trans-position relative to atom N(1). The Co–O(2)" distance (2.029 Å) is noticeably shorter than the other bond lengths, Co–O(Nta) (2.069–2.103 Å), Co–O(w1), and Co–N(1) (2.155 and 2.177 Å, respectively). Cations Ca2+are located in the inversion centers and involve in their coordination atoms O(4), O(6), O(w2), and the oxygen atoms symmetrically bond to them and arranged at 2.271(1), 2.420(1), and 2.351(2) Å, respectively. The structural formula of the title compound is {Ca(H2O)2[Co(Nta)(H2O)]2}3· 2H2O.  相似文献   

16.
The complex of 1,4,7,10,13-pentaoxacyclohexadecane-14,16-dione (L) with potassium thiocyanate, C11H18O7· KNCS (I), is prepared and characterized by X-ray diffraction analysis: space group C2/c, a = 26.810 Å, b = 7.834 Å, c = 20.504 Å, = 129.19°, Z = 8. The crystal structure is solved by the direct method and refined anisotropically by the full-matrix least-squares method to R = 0.038 for all 2929 unique measured reflections (CAD4 automated diffractometer, MoK ). Structure I is built of [KL(NCS)] monomers of the host–guest type, which are united into [K2L2(NCS)2] dimers containing four-membered KNKN cycles. In the crystal, the dimers are united into infinite polymeric double chains (along the b axis) by K···O=C outer bonds. The K+ cation (CN 8) does not lie in the plane of the L crown ligand but is located above it. The coordination polyhedron of the K+ cation is irregular; its vertices are occupied by five ether O atoms of one L ligand, two N atoms of two SCN ligands, and one carbonyl O atom of the adjacent L ligand.  相似文献   

17.
The aqua complex of podand 1,2-bis(2-(o-hydroxyphenoxy)ethyloxy)ethane (L) with strontium thiocyanate of the composition [Sr(NCS)L(H2O)2]+ · SCN (I), was synthesized and studied by X-ray diffraction analysis: space group P 21/c, a = 17.730 Å, b = 8.558 Å, c = 18.169 Å, = 116.15°, Z = 4. The structure was solved by direct method and anisotropically refined by the full-matrix least-squares method to R = 0.039 for 4333 independent reflections (CAD4 autodiffractometer, MoK ). Structure I contains complex cation [Sr(NCS)L(H2O)2]+ of the host–guest type. The coordination polyhedron of Sr2+ cation (coordination number 9) is a distorted pentagonal bipyramid with four oxygen atoms at the benzene rings of the L podand and the oxygen atom of one water molecule in its base, the N atom of the SCN ligand at its single vertex, and with the remaining two O atoms of the L podand and O atom of another water molecule at a triple vertex. In a crystal, the complex cations and SCN anions are joined through the hydrogen bonds to form bulky layers parallel to the xy plane.  相似文献   

18.
The crystal structure of thallium fluoroantimonate(III) complex TlSb4F13 (I), which is isostructural to KSb4F13 (II), is determined. Crystals I are tetragonal: a = 9.634(2) Å, c = 6.590(2) Å, V = 611.7(2) Å3, Z = 2, (calcd) = 5.094 g/cm3, F(000) = 804.0, space group I4¯. The structure consists of tetrameric [Sb4F13] anions formed by SbF3 groups connected by the fluoride ion and the l+ cations.  相似文献   

19.
Crystals of [Cu(DAF)(H2O)]BF4(I) and [Cu(DAF)(ClO4)] (II) (DAF is diallyl formamide) were synthesized by an alternate-current electrochemical method, and their structures were determined (MoK radiation, 1247 and 859 independent reflections with I 2(I), R= 0.043 and 0.032 for Iand II, respectively). The complexes crystallize in space group P21/n, Z= 4. For I, a= 10.782(3) Å, b= 12.096(5) Å, c= 9.185(3) Å, = 103.62(3)°, and V= 1164.2(7) Å3; for II, a= 10.064(3) Å, b= 10.753(6) Å, c= 10.002(3) Å, = 87.52(4)°, and V= 1081.4(8) Å3. The copper atom in structures Iand IIcoordinates both C=C bonds in one DAF molecule and oxygen atom of the amide group of another DAF molecule, as well as an oxygen atom of H2O (in I) or ClO4(in II) in the axial position. The uncommon behavior of the anions in structures Iand IIis explained by their different values of Pierson hardness.  相似文献   

20.
A complex of uranyl perchlorate with imidazolidine-2-one as the molecular ligand, [UO2(Imon)4(H2O)](ClO4)2 (I), was synthesized and structurally characterized by X-ray diffraction analysis. The coordination number of the uranium atom is 7. The nearest environment of the uranyl ion includes four O atoms of the imidazolidine-2-one molecules and one O atom of the water molecule. The perchlorate anions are outer-sphere ligands. The crystals are monoclinic: space group P21/c; a = 16.294(3) Å, b = 16.135(3) Å, c = 9.987(2) Å, = 97.69 (3)°, V = 2603.0 (9) Å3, (calcd) = 2.117 g/cm3, Z = 4. The IR and luminescence spectra of the complex were recorded.Translated from Koordinatsionnaya Khimiya, Vol. 30, No. 12, 2004, pp. 919–924.Original Russian Text Copyright © 2004 by Andreev, Antipin, Budantseva, Tuchina, Serezhkina, Fedoseev, Yusov.  相似文献   

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