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1.
The structure of [Pb3(OH)4Co(NO2)3](NO3)(NO2)·2H2O is determined by single crystal X-ray diffraction. The crystallographic characteristics are as follows: a = 8.9414(4) Å, b = 14.5330(5) Å, c = 24.9383(9) Å, V = 3240.6(2) Å3, space group Pbca, Z = 8. The Co(III) atoms have a slightly distorted octahedral coordination formed by three nitrogen atoms belonging to nitro groups (Co–Nav is 1.91 Å) and three oxygen atoms belonging to hydroxyl groups (Co–Oav is 1.93 Å). The hydroxyl groups act as μ3-bridges between the metal atoms. The geometric characteristics are analyzed and the packing motif is determined.  相似文献   

2.
The complex [Co(2-Me-Pyz)2(H2O)4](NO3)2 is synthesized and its structure is determined. The crystals are monoclinic: space group P21/n, a = 10.685(2) Å, b = 6.837(1), c = 12.515(3) Å, β = 91.84(3)°, V = 913.8(3) Å3, ρcalcd = 1.042 g/cm 3, Z = 2. The Co2+ ion (in the inversion center) is coordinated at the vertices of the distorted octahedron by two nitrogen atoms of methylpyrazine and four oxygen atoms of the water molecules (Co(1)–N(1) 2.180(3), average Co(1)–O(w) 2.079(3) Å, angles at the Co atom 87.9(1)–92.1(1)°). Supramolecular pseudometallocycles are formed in the structure through the O(w)–H…N(1) hydrogen bonds between the coordinated H2O molecules and the terminal nitrogen atoms of the 2-methylpyrazine molecules. Their interaction results in the formation of supramolecular layers joined by the NO3 groups into a three-dimensional framework.  相似文献   

3.
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) Å3, Z = 2, ρcalcd = 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.  相似文献   

4.
Interaction of Co(II) chloride with optically active bis-pinane propylenediaminodioxime (H2L) gave a diamagnetic compound of Co(III) with a composition [Co(HL)Cl2]. The crystal and molecular structure of the compound was determined by X-ray diffraction (XRD) analysis (Enraf-Nonius CAD-4 diffractometer, λMoKα, 703 F hkl , R = 0.0347). The crystals are orthorhombic with unit cell parameters a = 8.989(1) Å, b = 12.351(2) Å, c = 22.425(3) Å, V = 2487.7(6) Å3, Z = 4, ρcalc = 1.420 g/cm3, space group P212121. The crystal structure of the complex is composed of discrete one-center molecules. In the complex, the Co3+ ion coordinates four N atoms of the tetradentate cycle-forming ligand (HL? anion) and two Cl atoms. The coordination polyhedron of Co is a distorted octahedron Cl2N4.  相似文献   

5.
Vanadium(V) complexes of general composition M3VO2(SO4)2 (M = Rb, Cs) were synthesized by a solid-state route. The individuality of the synthesized compounds was proved by X-ray and neutron diffraction, vibrational spectroscopy, and microscopic analysis. The X-ray diffraction patterns of M3VO2(SO4)2 were indexed to fit the monoclinic system (space group P2/c, Z = 4) with the following unit cell parameters: a = 11.6487(2) Å, b = 8.4469(2) Å, c = 12.1110(2) Å, β = 109.483(1)°, V = 1123.43 Å3 (Rb); a = 12.0546(3) Å b = 8.7706(2) Å, c = 12.6496(3) Å, β = 109.843(2)°, V = 1257.99 Å3 (Cs). In the crystal structure of M3VO2(SO4)2, [VO2(SO4)2]3? complex anions can be discerned in which the vanadium atom is surrounded by five oxygen atoms: two oxygen atoms form short terminal V–O bonds, and three oxygen atoms are from the two sulfato groups, one of which acts as a monodentate ligand and the other acts as a bidentate chelating ligand.  相似文献   

6.
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) Å3, 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) Å3, 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) Å3, 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.  相似文献   

7.
The trans(O)-cis(C)-bis(pyridine-2-carboxylato)dicyanocobaltate(III) ions, [Co(Pic)2(CN)2]?, crystallize from acid medium with three water molecules per two crystallographically nonequivalent complexes whose charge is compensated by protons. One of the water molecules forms an oxonium ion (H3O+) with a proton. The other two water molecules bound to each other through a short hydrogen bond O-H…O (2.403(2) Å) and thus forming (H5O2)+ cations is another proton site. The (H3O)(H5O2)[Co(Pic)2(CN)2]2 crystals are monoclinic: a = 10.7027(7) Å, b = 25.786(1) Å, c = 11.4865(8) Å, β = 91.411(9)°, Z = 4, space group P21/n.  相似文献   

8.
Heteroligand complexes [Co2(HMTA)(iso-Bu2PS2)4] (I) (μeff = 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, ρcalcd = 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, ρcalcd = 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.  相似文献   

9.
Heating of a hydrochloric acid solution of trans-PtPy(NH2CH2CN)Cl4 results in the hydrolysis of coordinated aminoacetonitrile to aminoacetic acid with the formation of a five-membered chelate ring attached to platinum through the nitrogen atom of the amino group and the oxygen atom of the carboxy group. X-ray diffraction analysis of [PtPy(NH2CH2COO)Cl3] is carried out. The crystals are monoclinic: space group C2/c, a = 21.704(2), b = 8.7027(7), c = 15.576(1) Å, β = 126.606(1)o, V = 2361.8(3) Å3, Z = 8; R hkl = 0.057, wR = 0.141. In the neutral complex, the Pt atom has a distorted octahedral coordination. The equatorial plane is formed by a Cl atom (Pt-Cl, 2.284(3) Å), the N atom of the Py molecule (Pt-N, 2.062(8) Å), and the N and O atoms of the bidentate-chelating ligand (Pt-N, 2.039(8); Pt-O, 2.026(7) Å); two Cl atoms are arranged in the apical positions (Pt-Cl, 2.301(3) and 2.312(3) Å). The five-membered chelate ring has a flattened gauche conformation with an NCCO torsion angle of 19(1)°.  相似文献   

10.
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   

11.
The ligand 4,4′-bipyridyl-N,N′-dioxide (4,4′-dpdo) was used in the synthesis of two complexes, {Co(4,4′-dpdo)2[N(CN)2]2(H2O)2} (1) and {Mn(4,4′-dpdo)2[N(CN)2]2(H2O)2} (2). The complexes were found to be isostructural, triclinic, space group P-1 with Z = 1 and the following unit cell parameters: a = 8.158(8) Å, b = 8.865(8) Å, c = 9.477(9) Å; α = 70.988(13)°, β = 78.778(13)°, γ = 71.964(10)°; V = 612.8(10) Å3 for 1; a = 8.247(14) Å, b = 9.001(16) Å, c = 9.707(17) Å; α = 71.02(2)°, β = 78.63(2)°, γ = 72.62(2)°; V = 646(2) Å3 for 2. Final R-values were 0.075 and 0.083 for 1 and 2, respectively. In the molecules of the complexes, Co(II) or Mn(II) cation is coordinated by two O-atoms of two 4,4′-dpdo ligands, two terminal N-atoms of two dicyanamides, and two O-atoms of water molecules. The crystals are molecular, with adjacent complex molecules linked through a system of O-H...N and O-H...O hydrogen bonds.  相似文献   

12.
Triple phosphates A2FeTi(PO4)3 (A = Na, Rb) were synthesized by the solid-phase method and studied by electronic microscopy, electron probe X-ray microanalysis, and IR and Mössbauer spectroscopy. The crystal structure of the obtained compounds was refined by X-ray powder diffraction (the Rietveld method). The unit-cell parameters are as follows: for Na2FeTi(PO4)3 (space group R \(\overline 3 \) c, Z = 6), a = 8.6015(1) Å, c = 21.718(1) Å, V = 1391.52(1) Å3; for Rb2FeTi(PO4)3 (space group P213, Z = 4), a = 9.8892(2) Å, V = 967.12(1) Å3. The base of the crystal structures is a mixed octahedral-tetrahedral framework {[FeTi(PO4)3]2?}3∞. Na+ and Rb+ cations are arranged in cavities of the framework. The influence of cationic substitutions on the change of the structural type of the isoformular compounds A2FeTi(PO4)3 (A = Na, Rb) was considered.  相似文献   

13.
Polyiodides of acetamide complexes of transition elements have been synthesized and studied by X-ray diffraction analysis. Compounds [M(AA)6][I10] (M = Mn, Fe, Co, Ni, Zn) are isostructural with the earlier studied cadmium compound. The crystals of [Co(AA)4(H2O)2][I12] are monoclinic: a = 17.486(6) Å, b = 15.015(4) Å, c = 7.8309(15) Å, β = 99.87(2)°, V = 2025.6(10) Å3, space group C2/m, Z = 4. The crystals of [Ni(AA)6][I3]2 are monoclinic: a = 23.032(9) Å, b = 12.176(4) Å, c = 18.274(5) Å, β = 139.22(3)°, V = 3347.0(19) Å3, space group Cc, Z = 4.  相似文献   

14.
The crystals of a cluster complex of rhenium [{Cu(trien)}2Re4Te4(CN)12]· 3.5H2O were synthesized by the reaction of aqueous K4[Re4Te4(CN)12] with an aqueous ammonia solution of copper chloride in the presence of a polydentate ligand triethylenetetraamine (trien). The structure of the compound was established by X-ray single crystal analysis (a = 14.2617(11) Å, b = 15.7220(7) Å, c = 21.8554(16) Å, β = 98.554(2)°, V = 4846.0(6) Å3, Z = 4, space group P21/n, R = 0.0436). Two copper cations in the complex are coordinated to one cluster anion [Re4Te4(CN)12]4?. The copper atoms have typical five-coordinated surroundings formed by the nitrogen atom of the bridging cyanide ligand and four amino groups of the tetradentate trien.  相似文献   

15.
Two coordination compounds of compositions [Ni(L1)(idba)(H2O)]·1.5 H2O (1) and [Ni(L2)Fe(CN)5NO]·C2H5OH (2) where L1 is N, N′-bis(3-aminopropyl)ethylenediamine, L2 is 2,12-dimethyl-3,7,11,17-tetraazabicyclo[11.3.1]heptadeca-1(17),2,11,13,15-pentaene, and idba2? is 2,2′-iminodibenzoate have been synthesized and characterized by elemental analysis, IR spectroscopy, thermal analysis, and single-crystal X-ray diffraction. Complex 1 crystallizes in the monoclinic space group P21/n (No. 14) with a=9.810(2) Å, b=10.230(2) Å, c=25.350(5) Å, V=2543.6(9) Å3, Z=4, and R=0.0727. The nickel atom is six-coordinated by four N atoms of amine and two O atoms of water and idba2?. The molecular packing of the complex comprises of an infinite one-dimensional layered network in which the molecules in the crystal are held together by a system of hydrogen bonding. Complex 2, however, crystallizes in the space group C2/c (No. 15) of the monoclinic system with a=19.7990(4) Å, b=14.9440(3) Å, c=19.8800(3) Å, V=5115.90(17) Å3, Z=4, and R=0.0540. The Ni ion in compound 2 has a slightly distorted octahedral arrangement of the N4 donor atoms of primary ligand L2 and two N-donor atoms of the secondary nitroprusside ligand. The structure of 2 displays an extended one-dimensional network formed by linear [—Ni—NC—Fe—CN—] units. A cyclic voltammetric study shows that compound 1 undergoes a quasireversible oxidation attributable to Ni2+ → Ni3+ in the range 300–420 mV vs SCE.  相似文献   

16.
The crystal structure of KLaMo(CN)8 · 9H2O was determined from X-ray diffraction data. The crystals are monoclinic, space group P21/c, a = 8.7451(4), b = 25.2761(13), c = 10.6744(5) Å, β = 117.059(3)°, V = 2101.22(17) Å3, Z = 4, ρ(calcd) = 2.037 g/cm3, R = 0.0242, wR 2 = 0.0500 for 5656 independent reflections. The coordination polyhedra of the Mo, La, and K atoms are the tetragonal antiprism [Mo(CN)8], the monocapped tetragonal antiprism [La(NC)4(OH2)5], and the strongly distorted monocapped trigonal prism [K(NC)3(OH2)4], respectively. The La and K atoms are N-linked by seven bridging cyano groups to form double layers with two sandwiched uncoordinated water molecules and the sandwiched terminal CN group. The complex can be formulated as “[K(H2O)2][La(H2O)5][Mo(CN)8]” n · 2nH2O.  相似文献   

17.
Crystals of Ba[Co(Nta)(C2O4)] · 3H2O were prepared, and their structure was solved by X-ray diffraction (monoclinic space group P21/c), a = 10.0111(10) Å, b = 10.2838(6) Å, c = 14.2748(15) Å, ß = 100.350(12)°, Z = 4). The local environment of a Ba2+ ion includes two O atoms of water molecules and seven O atoms of the carboxyl groups of Nta3? and C2O 4 2? ions of five complex anions. Honeycomb type layers can be distinguished in the crystal lattice; within the layers, each Ba2+ atom interacts with three complexes and vice versa. In addition, each Ba atom of the layer is bonded to complexes of the upper and lower layers. Thus, the crystal represents a three-dimensional coordination polymer.  相似文献   

18.
Compound [Zn(CF3CO2)2(Bpp)2], where Bpp is 1,3-bis(4-pyridyl)propane, was synthesized and its structure and luminescent properties were determined. Crystals are monoclinic, space group C2/c, a = 21.261(1) Å, b = 17.642(1) Å, c = 18.632(1) Å, β = 115.85(1)°, V = 6289.3(6) Å3, ρcalcd = 1.453 g/cm3, Z = 8. The structure comprises 2D neutral layers of conjugated multiunit rings composed of four Zn2+ ions united by four bridging Bpp ligands. Each of two crystallographically nonequivalent Zn atoms is coordinated at the octahedra apices to four nitrogen atoms of two Bpp ligands and two O(CF3CO2) atoms. Trifluoroacetate anions are coordinated to Zn2+ ions in monodentate manner. The compound exhibits photoluminescence in solid state.  相似文献   

19.
The products of 4′,5′-dibromobenzo-15-crown-5 (I) cyanation by the Rosenmund-Braun reaction are studied by the 1H NMR and IR spectroscopy methods. X-ray diffraction analysis of two isolated products, i.e., di(4′,5′-dicyanobenzo-15-crown-5) 1.6 hydrate {(CN)2B15C5}2 · 1.6H2O (IIa) and 4′,5′-dicyanobenzo-15-crown-5,4′-cyano-5′-cyano(bromo)benzo-15-crown-5 dihydrate (CN)3.85Br0.15(B15C5)2 · 2H2O (III) is performed. Crystals IIa are monoclinic, a = 15.882(2) Å, b = 11.412(2) Å, c = 18.484(3) Å, β = 100.717(3)°, V = 3291.7(9) Å3, Z = 4, space group P21/c, R = 0.0746 for 4775 reflections with I > 2σ(I). Crystals III are monoclinic, a = 15.956(3) Å, b = 11.425(2) Å, c = 18.865(4) Å, β = 99.32(3)°, V = 3394(1) Å3, Z = 4, space group P21/c, R = 0.0692 for 2070 reflections with I > 2σ(I). Compounds IIa and III have similar structures with two crystallographically independent molecules in each (A and B in IIa; C and D in III). Four of the five O atoms of a macrocycle in molecules A and C form hydrogen bonds with the water molecules. The latter molecules lie above and below the cycle plane at a distance of ~2 Å from this plane. The A and C molecules have identical conformations (TTG TTG TTG TTG TTC) that differ from those of molecules B (TTG TGG STT SSG TTC) and D (TTC TSG STT SSG TTC).  相似文献   

20.
The syntheses and crystal structures of the layered coordination polymers M(C8H8NO2)2 [M = Mn (1), Co (2), Ni (3) and Zn (4)] are described. These isostructural compounds contain centrosymmetric trans-MN2O4 octahedra as parts of infinite sheets; the ligand bonds to three adjacent metal ions in μ3-N,O,O′ mode from both its carboxylate O atoms and its amine N atom. In each case, weak intra-sheet N–H?O and C–H?O hydrogen bonds may help to consolidate the structure. Crystal data: 1, C16H16MnN2O4, M r = 355.25, monoclinic, P21/c (No. 14), a = 10.6534(2) Å, b = 4.3990(1) Å, c = 15.5733(5) Å, β = 95.1827(10)°, V = 726.85(3) Å3, Z = 2, R(F) = 0.026, wR(F 2) = 0.067. 2, C16H16CoN2O4, M r = 359.24, monoclinic, P21/c (No. 14), a = 10.6131(10) Å, b = 4.3374(4) Å, c = 15.3556(17) Å, β = 95.473(4)°, V = 703.65(12) Å3, Z = 2, R(F) = 0.041, wR(F 2) = 0.091. 3, C16H16N2NiO4, M r = 359.02, monoclinic, P21/c (No. 14), a = 10.6374(4) Å, b = 4.2964(2) Å, c = 15.2827(8) Å, β = 95.9744(14)°, V = 694.66(6) Å3, Z = 2, R(F) = 0.028, wR(F 2) = 0.070. 4, C16H16N2O4Zn, M r = 365.68, monoclinic, P21/c (No. 14), a = 10.6385(5) Å, b = 4.2967(3) Å, c = 15.2844(8) Å, β = 95.941(3)°, V = 694.89(7) Å3, Z = 2, R(F) = 0.038, wR(F 2) = 0.107.  相似文献   

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