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1.
A. N. Chekhlov 《Russian Journal of Coordination Chemistry》2009,35(6):464-467
A new complex [K(Db18C6)]+[FeCl4]? (I) is synthesized and its structure is studied by X-ray diffraction analysis. The crystals are triclinic: space group P \(\bar 1\), a = 17.998, b = 18.670, c = 19.590 Å, α = 106.61°, β = 104.55°, γ = 113.87°, 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 = 0.057 by 13 670 independent reflections (CAD-4 automated diffractometer, λMoK α). All the four independent complex cations [K(Db18C6)]+ are host-guest, and in each complex cation the K+ cation is localized in the cavity of the Db18C6 crown ligand. The coordination polyhedron of K+ (coordination number nine) is a distorted hexagonal bipyramid with the base of all six O atoms of the Db18C6 ligand, the axial vertex at the Cl atom of the [FeCl4]? anion, and another bifurcated axial vertex at two Cl atoms of another [FeCL4]? anion. All the four independent [FeCL4]? anions are orientationally disordered and have somewhat distorted tetrahedral structure. In crystal I, the alternating complex cations [K(Db18C6)]+ and [FeCL4]? anions form infinite polymer chains by the K-Cl bonds. 相似文献
2.
A. N. Chekhlov 《Russian Journal of Coordination Chemistry》2009,35(3):222-225
A new complex [Cs(Db18C6)2]+[FeCl4]? was prepared and studied by X-ray diffraction (orthorhombic, space groupP21212,a = 22.934 Å,b= 24.024 Å,c= 16.665 Å,Z= 8; direct method, anisotropic full-matrix least-squares refinement,R= 0.087 for all 8800 independent reflections; CAD4 automated diffractometer, λMoK α. Two independent [FeCl4]? anions have a slightly distorted tetrahedral structure. Two independent host-guest type complex cations [Cs(Db18C6)2]+ have a sandwich structure. The Cs+ cation is located between two Db18C6 crown ligands below and above the centers of their 18-membered macrocycles and is coordinated by all 12 O atoms. The coordination polyhedron of Cs+ (C.N. 12) is a distorted hexagonal antiprism rotated toward a hexagonal prism. 相似文献
3.
A. N. Chekhlov 《Russian Journal of Inorganic Chemistry》2010,55(3):390-394
A new compound, (dibenzo-18-crown-6)ammonium bromide tetrahydrofuran solvate [NH4(Db18C6)]+ · Br? · THF (I), is synthesized and studied by X-ray diffraction analysis. The crystals of compound I are triclinic: a = 8.848 Å, b = 9.696 Å, c = 16.023 Å, α = 73.75°, β = 86.93°, γ = 78.06°, Z = 2, space group P \(\bar 1\). The structure of compound I is solved by a direct method and refined by full-matrix least squares in the anisotropic approximation to R = 0.095 by 5624 independent reflections (CAD-4 automated diffractometer, γMoK α). The Db18C6 molecule in structure I has a butterfly conformation with approximate symmetry C 2v . The NH 4 + cation where three disordered H atoms form hydrogen bonds with all six O atoms of the Db18C6 molecule is situated in the center of the cavity of the eighteen-membered macrocycle of the Db18C6 molecule. One ordered H atom of the NH 4 + cation forms a strong hydrogen bond with the Br? anion. 相似文献
4.
A. N. Chekhlov 《Russian Journal of Inorganic Chemistry》2008,53(8):1197-1202
Two crystalline host-guest complexes are synthesized and studied using X-ray diffraction analysis: (18-crown-6)sodium tribromide [Na(18-crown-6)]+ · Br 3 ? (I) and (18-crown-6)potassium tribromide (with an admixture of bromodiiodide) [K(18-crown-6)]+ · (Br0.25I2.75)? (II). The structures of compound I (space group P21/n, a = 8.957 Å, b = 8.288 Å, c = 14.054 Å, β = 104.80°, Z = 2) and compound II (space group Cc, a = 8.417 Å, b = 15.147 Å, c = 17.445 Å, β = 99.01°, Z = 4) are solved by a direct method and refined by the full-matrix least-squares method in the anisotropic approximation to R = 0.098 (I) and 0.036 (II) for all 2311 (I) and 2678 (II) independent measured reflections on a CAD-4 automated diffractometer (λMoK α). Similar crystalline complexes I and II exist as infinite chains of alternating complex cations and trihalide anions linked to each other through weak Na-Br or K-I coordination bonds. In [Na(18-crown-6)]+ and [K(18-crown-6)]+ complex cations, the Na+ or K+ cation (coordination number is eight) is located in the center of the cavity of the 18-crown-6 ligand and coordinated by the six O atoms and two terminal Br or I atoms of two trihalide anions lying on opposite sides of the rms plane of the crown ligand. 相似文献
5.
A. N. Chekhlov 《Russian Journal of Inorganic Chemistry》2010,55(1):82-86
The crystal structure of (ethoxycarbonylmethyl)triphenylphosphonium tetrafluoroborate, Ph3P+CH2C(O)OEt · BF 4 ? (space group P21/n, a = 12.727 Å, b = 13.983 Å, c = 12.833 Å, β = 108.83°, Z = 4) is studied by single-crystal X-ray diffraction. The structure was solved by a direct method and refined by full-matrix least squares in the anisotropic approximation to R = 0.056 by 3200 independent reflections (CAD-4 automated diffractometer, λMoK α). In the phosphonium cation the P atom has a distorted tetrahedral coordination and the P-C-C=O torsion angle is 14.3°. The tetrahedral anion is slightly disordered over two orientations with site occupancies for all atoms of 0.875 and 0.125. The crystal contains unusual interionic hydrogen bonds of the P+-C-H…F-B? type. 相似文献
6.
Potassium bis(malonato)borate C6H4BKO8 (I) was synthesized for the first time in an aqueous medium. Well-shaped single crystals were formed. Their X-ray diffraction structure (space group P \(\overline 1 \), a = 7.4073(2) Å, b = 7.9161(2) Å, c = 9.0755(2) Å, α 113.225(1)°, β = 91.553(1)°, γ = 104.760(2)°, Z = 2) was refined by the full-matrix least-squares method in the anisotropic (K, C, O, B) or isotropic (H) approximations to R1 = 0.394, wR2 = 0.1080, 2661 independent reflections (Bruker-Nonius KappaCCD, λMoK α radiation). The structure is formed by spirane-type complex anions and potassium cations. A complex anion consists of two malonic acid molecules coordinated in the bidentate mode to the same four-coordinate boron atom. The K+ coordination geometry is an irregular nine-vertex polyhedron formed by the oxygen atoms of seven complex anions. The structure of compound I is layered. 相似文献
7.
P. A. Stabnikov L. G. Bulusheva N. I. Alferova A. I. Smolentsev I. A. Korol’kov N. V. Pervukhina I. A. Baidina 《Journal of Structural Chemistry》2012,53(4):740-747
Crystal structures are determined (Bruker Nonius X8 Apex, 4K CCD-detector, λMoK α, graphite monochromator, T 150 K and 293 K) for two β-diketones F3CC(O)CH2C(O)Ph (1) (space group P21/c, a = 7.0713(3)Å, b = 11.5190(6)Å, c = 11.3602(6) Å, β = 99.405(2)°, V = 912.90(8) Å3, Z = 4), (CH3)3CC(O)CH2C(O)C(CH3)3 (2) (space group Pbca, a = 11.5536(8) Å, b = 11.5796(10) Å, c = 17.2523(13) Å, V = 2308.1(3) Å3, Z = 8) and a ketoimine (CH3)3CC(NCH3)CH2C(O)C(CH3)3 (3) (space group I41/a, a = 18.7687(6) Å, b = 18.7687(6) Å, c = 14.5182(6) Å, V = 5114.2(3) Å3, Z = 16). All structures are molecular and comprise isolated molecules joined by van der Walls interactions. The substitution energy of a Na atom for a hydrogen atom in free ligands is calculated by the hybrid B3LYP quantum chemical method. A successful preparation of Na(I) chelates with ligands 1, 2 and failed attempts to prepare a complex with ligand 3 are in accordance with the calculations. Geometrical simulation of a copper(II) complex with ligand 3 reveals the overlap of CH3 groups which hinders the complexation. 相似文献
8.
A. N. Chekhlov 《Russian Journal of Coordination Chemistry》2009,35(7):492-495
The new complex [Sr(18-crown-6)(H2O)3]2+[CuCl4]2? · 0.42H2O was obtained; its crystal structure was determined by X-ray diffraction analysis: space group P21, a = 10.305 Å, b = 13.570 Å, c = 17.566 Å, β = 98.23 °, Z = 4 (direct method, anisotropic full-matrix least-squares method, R = 0.053 from independent reflections; CAD-4 automated diffractometer, λMoK α). The asymmetric part of the unit cell comprises two independent “guest-host” complex cations [Sr(18-crown-6)(H2O)3]2+, two independent complex anions [CuCl4]2?, and a hydrate water molecule with a position population of 0.84(1). 相似文献
9.
A. N. Chekhlov 《Russian Journal of Coordination Chemistry》2005,31(12):861-865
A novel complex salt, namely, 4,7,13,16,21,24-hexaoxa-1,10-diazoniabicyclo[8.8.8]hexacosane bis[dibromodichloroiron(III)] [H2(Crypt-222)]2+[FeBr2Cl2] 2 ? (I), was synthesized and structurally characterized by X-ray diffraction analysis (monoclinic crystal system, a = 13.550 Å, b = 11.018 Å, c = 12.813 Å, β = 117.52°, space group C2, Z = 2). The structure was solved by the direct method and refined by the full-matrix least-squares method in the anisotropic approximation to R = 0.089 from 2593 independent reflections (CAD4 automated diffractometer, λMoKα radiation). In the crystal structure I, four bifurcate positions of Br and Cl in the tetrahedral anion [FeBr2Cl2]? are a randomly disordered mixture of these atoms. The dication of 2.2.2-cryptand (with two protonated N atoms) in the crystallographic axis 2 contains trifurcate N+-H (?O)3 hydrogen bonds. 相似文献
10.
A. N. Chekhlov 《Russian Journal of Inorganic Chemistry》2010,55(7):1107-1111
A 3: 1: 1 crystalline adduct of orthophosphoric acid, crown ether dibenzo-18-crown-6, and water, 3H3PO4 · Db18C6 · H2O (I), is synthesized and studied by X-ray diffraction analysis. The orthorhombic structure of compound I (space group Pmn21, a = 23.123 Å, b = 12.595 Å, c = 4.922 Å, Z = 2) is solved by a direct method and refined by full-matrix least squares in the anisotropic approximation to R = 0.061 by all 1894 independent reflections. One H3PO4 molecule and Db18C6 and H2O molecules lie on the crystallographic plane m. The H3PO4 molecules are randomly disordered. The H atoms of the H3PO4 and H2O molecules are not objectively revealed because of high disordering. The Db18C6 and H2O molecules form the host-gust molecular complex [Db18C6 · H2O] through hydrogen bonds. All H3PO4 molecules are hydrogenbonded to form infinite layers lying parallel to the xz plane. The [Db18C6 · H2O] molecular complexes are arranged between the layers. 相似文献
11.
A. N. Chekhlov 《Russian Journal of Inorganic Chemistry》2008,53(9):1470-1475
Two complexes with similar compositions are synthesized: (18-crown-6)(nitrato-O,O′)potassium (I) and (18-crown-6)(nitrato-O,O′)potassium(0.91)silver(0.09) (II). Their isomorphic orthorhombic crystals (space group P212121, Z = 4) are studied by X-ray diffraction analysis. Structure I (a = 8.553 Å, b = 11.967 Å, c = 17.871 Å) and structure II (a = 8.540 Å, b = 11.956 Å, c = 17.867 Å) are solved by a direct method and refined by the full-matrix least-squares method in the anisotropic approximation to R = 0.044 (I) and 0.055 (II) for all 2385 (I) and 2379 (II) measured independent reflections. Complex molecules [K(NO3)(18-crown-6)] in structure I and [K0.91Ag0.09(NO3)(18-crown-6)] in compound II are of the host-guest type and rather similar in structure. Their 18-crown-6 and NO 3 ? ligands are disordered over two orientations. The K+ cation in complex I and the mixed cation (K0.91Ag0.09)+ in complex II reside in the cavity of the disordered 18-crown-6 ligand and is coordinated by its six O atoms and by two disordered O atoms of the NO 3 ? . ligand. The coordination polyhedron (CN = 8) of the K+ cation in complex I and that of (K0.91Ag0.09)+ cation in complex II is a distorted hexagonal pyramid with a base of six O atoms of the 18-crown-6 ligand and a split vertex at two O atoms of the NO 3 ? ligand. 相似文献
12.
A. N. Chekhlov 《Russian Journal of Coordination Chemistry》2009,35(8):628-631
A new complex K(18-crown-6)][Dy(NO3)4(H2O)2] · CH3CN (I) is synthesized, and its structure is studied by X-ray diffraction analysis (space group P 21/c, a = 17.200 Å, b = 13.377 Å, c = 13.087 Å, β = 94.21°, Z = 4, full-matrix anisotropic least squares to R = 0.033 for 5283 independent reflections, CAD-4 automated diffractometer, λMoKα radiation). The crystal structure of the compound exists as infinite polymer chains formed by coordination bonds and composed of alternating complex anions [Dy(NO3)4(H2O)2]? and cations [K(18-crown-6)]+. 相似文献
13.
A. N. Chekhlov 《Russian Journal of Inorganic Chemistry》2007,52(12):1918-1924
Two complexes, namely, triaqua(18-crown-6)strontium dibromide monohydrate (I) and diaquabromo(18-crown-6)barium bromide (II), are synthesized. Their crystal structures are determined by X-ray diffraction analyses. For complex I, space group C2/c, a = 17.547 Å, b = 10.246 Å, c = 14.786 Å, β = 123.08°, Z = 4. For complex II, space group Pnma, a = 17.753 Å, b = 17.465 Å, c = 6.629 Å, Z = 4. The structures are solved by a direct method and refined by the full-matrix least-squares method in the anisotropic approximation to R = 0.056 (I) and 0.042 (II) for 2696 (I) and 2440 (II) independent reflections (CAD-4 automated diffractometer, λMoK α radiation). Both complex cations—randomly disordered [Sr(18C6)(H2O)3]2+ in complex I and [BaBr(18C6)(H2O)2]+ in complex II—are of the host-guest type. The Sr2+ (Ba2+) cation resides in the cavity of the 18-crown-6 ligand and coordinated by all six O atoms. In the structures complexes I and II, the coordination polyhedra of the Sr2+ and Ba2+ cations (coordination number 9) can be described as distorted hexagonal bipyramids with one apex at the O atom of the water molecule in complex I or at the Br? ligand in complex II and the other split apex at the O atoms of two water molecules. 相似文献
14.
A. N. Chekhlov 《Russian Journal of Coordination Chemistry》2007,33(1):32-36
A new complex salt [4,7,13,16,21,24-hexaoxa-1,10-diazoniabicyclo[8.8.8]hexacosane bis[dichloro(thiocyanato)copper(II)], [H2(Crypt-222)][CuCl2(SCN)]2, is synthesized and studied by X-ray diffraction analysis. The crystals are monoclinic (space group C2/c, a = 14.603 Å, b = 8.330 Å, c = 25.091 Å, β = 100.76°, Z = 4). The structure is solved by a direct method and refined by the full-matrix least-squares method in the anisotropic approximation to R = 0.047 for 2943 independent reflections (CAD-4 automated diffractometer, λMoK α radiation). The Cu2+ cations and Cl? and SCN? anions form infinite polymeric chains of spiro-conjugated alternating centrosymmetric four-membered CuCl2Cu cycles and eight-membered Cu(SCN)2Cu cycles through coordination bonds. The coordination polyhedron of the Cu2+ cation is a distorted trigonal bipyramid. The [H2(Crypt-222)]2+ dication contains trifurcate N+-(…O)3 bonds on axis 2. 相似文献
15.
The crystal structure of bis(semicarbazido)copper(II) nitrate [Cu(NH2NHC(O)NH2)2](NO3)2 has been studied by X-ray diffraction. Monoclinic crystals, a = 6.835(2) Å, b = 7.733(2) Å, c = 10.320(3) Å, β = 105.701(3)°, V = 525.1(2) Å3, space group P21/c, Z = 2, d
msd = 2.136 g/cm3, μ(MoK
α) = 2.143 mm−1. The structure was solved with the program for automatic analysis of Patterson’s function and refined by full-matrix least
squares in an anisotropic approximation for all non-hydrogen atoms using 753 independent reflections; R
1 = 0.0203. The square environment of the Cu atom is formed from the amino nitrogen atoms of the hydrazine fragments and the
C=O oxygen atoms of the two semicarbazide bidentate molecules (Cu-N 1.928 Å, Cu-O 1.999 Å). The axial positions are occupied
by the O atoms of the NO
3
−
outer-spheric anions (Cu-O 2.505 Å). In the structure, the complex cations and the NO
3
−
anions are linked into a framework by N-H...O type hydrogen bonds.
Original Russian Text Copyright ? 2007 by G. V. Romanenko, Z. A. Savelieva, and S. V. Larionov
__________
Translated from Zhurnal Strukturnoi Khimii, Vol. 48, No. 2, pp. 370–373, March–April, 2007. 相似文献
16.
A. N. Chekhlov 《Russian Journal of Coordination Chemistry》2005,31(11):823-827
A new complex (18-crown-6)(nitrato)(triphenylphosphine oxide)potassium (I) is synthesized, and its crystal structure is studied by X-ray diffraction analysis (space group R3m, a = 14.336 Å, c = 13.776 Å, Z = 3). The structure is solved by the direct method and refined by the full-matrix least-squares method in the anisotropic approximation to R = 0.034 for 1122 independent reflections (CAD4 automated diffractometer, λ MoKα radiation). Structure I contains a complex host-guest molecule [K(NO3)(18-crown-6)(Ph3PO)] with crystallographic symmetry 3m (three planes m contain three Ph rings of the Ph3PO ligand and all O atoms of the crown ligand). The coordination polyhedron of the K+ cation is a distorted hexagonal bipyramid with all the six O atoms of the crown ligand in the base, the O atoms of the Ph3PO ligand, and one (or two) O atoms of a disordered NO 3 ? ligand in the axial positions. 相似文献
17.
N. N. Golovnev M. S. Molokeev M. K. Lesnikov S. N. Vereshchagin 《Russian Journal of Inorganic Chemistry》2017,62(6):746-750
The lithium(I) catena-diaquabarbiturate complex [Li(H2O)2(HBA–O,O′)] n (I), where Н2ВА is barbituric acid, has been structurally characterized by X-ray diffraction (CIF file CCDC no. 1447689), and its thermal decomposition and IR spectrum have been studied. Crystals of complex I are monoclinic, a = 6.4306(7) Å, b = 16.720(1) Å, c = 7.1732(8) Å, β = 108.253(4)°, V = 732.5(1) Å3, space group P21/c, and Z = 4. One independent μ2-bridging HBA– ligand is coordinated to two Li(I) ions via the two oxygen atoms of C4(6)=O carbonyl groups. Each Li+ ion is linked with two μ2-HBA– ions and two terminal water molecules at tetrahedron vertices. μ2-HBA– ions link tetrahedra into a chain. The structure is stabilized by multiple hydrogen bonds and π–π-interaction between HBA–. The shift of ν(C=O) vibration bands in the IR spectrum of complex I in comparison with Н2ВА towards lower frequencies agrees with the coordination of HBA– via oxygen atoms. The dehydration of complex I occurs in two stages in the regions of 100–150 and 150–240°C. 相似文献
18.
Two phenanthroline-manganese inclusion complexes with [MnCl(H2O)(phen)2]+ core have been synthesized and characterized by single crystal X-ray diffraction, elemental analyses, IR spectra, thermogravimetric analyses. Uncoordinated 2-mercaptothiazole (tzdtH) and 2-mercaptobenzothiazole (bztzH) as guest molecules are included in the complexes with formulas [MnCl(H2O)(phen)2]Cl·tzdtH (1) and {[MnCl(H2O)(phen)2]Cl}2·bztzH (2). X-ray structural analyses for complexes revealed that the complex 1 is triclinic, space group P1 with a=9.724(1) Å, b=11.858(1) Å, c=12.644(2) Å; β=89.056(2)°; Z=2, D c=1.513 Mg m?3, F(000)=638 and the complex 2 is triclinic, space group P1 with a=9.861(1) Å, b=11.476(1) Å; c=12.908(3) Å; β=84.991(2)°; Z=1, D c=1.511 Mg m?3, F(000)=600. Two complexes exhibit high stability up to 650°C. The molar specific heat capacities for the two complexes 1 and 2 can be estimated as being 96.175±0.332 and 72.505±0.364 J mol?1 K?1 at 298.15 K by RD496-III microcalorimeter, respectively. 相似文献
19.
T. G. Cherkasova I. Yu. Bagryanskaya N. V. Pervukhina N. V. Kurat’eva V. V. Medvedev E. S. Tatarinova E. V. Cherkasova 《Russian Journal of Inorganic Chemistry》2017,62(6):760-765
New double complexes [Co(DMSO)6][SiF6] ? 2H2O (I) and [Co(DMF)3(H2O)3][SiF6] ? DMF (II) have been synthesized and studied by IR spectroscopy and X-ray diffraction. Crystals of complex I belong to the tetragonal symmetry system, space group R3?, Z = 3, a = 11.8232(3) Å, c = 18.4699(5) Å, V = 2235.97(10) Å3, ρcalc = 1.573 g/cm3. Crystals of complex II are triclinic, space group P1?, Z = 2, a = 8.6264(4) Å, b = 10.1419(4) Å, c = 13.9657(6) Å, α = 100.847(2)°, β = 98.549(2)°, γ = 93.479(2)°, V = 1181.71(9) Å3, ρcalc = 1.539 g/cm3. 相似文献
20.
A. N. Chekhlov 《Russian Journal of Inorganic Chemistry》2009,54(2):280-286
Two new complexes were synthesized, namely, 7: 2 (2.2.2-cryptand)potassium chloride and (2.2.2-cryptand)ammonium bromide(0.75)chloride(0.25) hydrates: [M(Crypt-222)]+ · Hal? · 3.5H2O, where M = K, Hal = Cl (I) and M = NH4, Hal = Br0.75Cl0.25 (II). The structures of two isomorphous crystals were studied by X-ray diffraction analysis. Trigonal (space group P \(\bar 3\), Z = 2) structures I (a = 11.763 Å, c = 11.262 Å) and II (a = 11.945 Å, c = 11.337 Å) were solved by direct methods and refined by the full-matrix least-squares method in the anisotropic approximation to R = 0.057 (I) and 0.065 (II) for all 2626 (I) and 1654 (II) independent measured reflections (CAD-4 automated diffractometer, λMoK α). In structures I and II, the host-guest [M(Crypt-222)]+ complex cation lies on the threefold crystallographic axis and has the approximate D 3 symmetry. In complex I, the coordination polyhedron of the K+ cation (CN = 8) is a bicapped trigonal prism somewhat distorted toward an antiprism. Complexes I and II contain H-bonded disordered cubes of the water molecules and the Cl? or Br? anions. 相似文献