Synthesis, Characterization and Crystal Structure of [Na2(APZC)2(μ-H2O)2(μ3-H2O)]n

The synthesis and spectroscopic properties of a Na^＋ complex with ligand 3-aminopyrazine-2-carboxylic acid were described. The resulting complex was characterized by elemental analysis, IR, UV-Vis, NMR spectroscopy and single crystal X-ray diffraction method. The title compound crystallizes in the triclinic system with space group . The crystalline structure of this compound consists of supramolecular architectures involving strong intramolecular N—H…O in pyrazine molecules and intermolecular O—H…N, O—H…O, and N—H…N hydrogen bonds between substituted pyrazine and water molecules.     

Crystal structures of seven-coordinate (NH4)2[MnII(edta)(H2O)]·3H2O, (NH4)2[MnII(cydta)(H2O)]·4H2O and K2[MNII(hdtpa)]·3.5H2O complexes

The title compounds, (NH₄)₂[Mn^II(edta)(H₂O)]·3H₂O (H₄edta = ethylenediamine-N,N,N′,N′-tetraacetic acid), (NH₄)₂[Mn^II(cydta)(H₂O)]·4H₂O (H₄cydta = trans-1,2-cyclohexanediamine-N,N,N′,N′-tetraacetic acid) and K₂[Mn^II(Hdtpa)]·3.5H₂O (H₅dtpa = diethylenetriamine-N,N,N′,N″,N″-pentaacetic acid), were prepared; their compositions and structures were determined by elemental analysis and single-crystal X-ray diffraction technique. In these three complexes, the Mn²⁺ ions are all seven-coordinated and have a pseudomonocapped trigonal prismatic configuration. All the three complexes crystallize in triclinic system in P-1 space group. Crystal data: (NH₄)₂[Mn^II(edta)(H₂O)]·3H₂O complex, a = 8.774(3) ?, b = 9.007(3) ?, c = 13.483(4) ?, α = 80.095(4)°, β = 80.708(4)°, γ = 68.770(4)°, V = 972.6(5) ?³, Z = 2, D _c = 1.541 g/cm³, μ = 0.745 mm⁻¹, R = 0.033 and wR = 0.099 for 3406 observed reflections with I ≥ 2σ(I); (NH₄)₂[Mn^II(cydta)(H₂O)]·4H₂O complex, a = 8.9720(18) ?, b = 9.4380(19) ?, c = 14.931(3) ?, α = 76.99(3)°, β = 83.27(3)°, γ = 75.62(3)°, V = 1190.8(4)?³, Z = 2, D _c = 1.426 g/cm³, μ = 0.625 mm⁻¹, R = 0.061 and wR = 0.197 for 3240 observed reflections with I ≥ 2σ(I); K₂[Mn^II(Hdtpa)]·3.5H₂O complex, a = 8.672(3) ?, b = 9.059(3) ?, c = 15.074(6) ?, α = 95.813(6)°, β = 96.665(6)°, γ = 99.212(6)°, V = 1152.4(7) ?³, Z = 2, D _c = 1.687 g/cm³, μ = 1.006 mm⁻¹, R = 0.037 and wR = 0.090 for 4654 observed reflections with I ≥ 2σ(I). Original Russian Text Copyright ? 2008 by X. F. Wang, J. Gao, J. Wang, Zh. H. Zhang, Y. F. Wang, L. J. Chen, W. Sun, and X. D. Zhang The text was submitted by the authors in English. Zhurnal Strukturnoi Khimii, Vol. 49, No. 4, pp. 753–759, July–August, 2008.     

Synthesis, structure, and thermal decomposition of [H2(4,4′-Bipy)][In(H2O)2(NCS)4]2 and [HUr]2[In(H2O)(NCS)5] · 2H2O

The reaction of indium thiocyanate with bipyridine (4,4-Bipy) and urotropine (Ur) gave [H₂(4,4′-Bipy)][In(H₂O)₂(NCS)₄]₂ (I) and [HUr]₂[In(H₂O)(NCS)₅] · 2H₂O (II), which were identified using elemental analysis, IR spectra, and thermogravimetric analysis. The thermal decomposition of compound I and II ends at 650 and 640°C, respectively, and gives In₂O₃. X-Ray diffraction analysis of compound I showed that complex anions in the crystal form chains through O-H…S hydrogen bonds. The anion chains form a close packing of columns with bipyridine cations located in the voids. Original Russian Text ? S.P. Petrosyants, A.B. Ilyukhin, V.A. Ketsko, 2008, published in Zhurnal Neorganicheskoi Khimii, 2008, Vol. 53, No. 6, pp. 951–955.     

Synthesis and Crystal Structure of (H)2[Y(H2O)8]2(NO3)8(C36H36N24O12)?13H2O

The compound of (H)₂[Y(H₂O)₈]₂(NO₃)₈(C₃₆H₃₆N₂₄O₁₂)13H₂O composition was obtained from a nitric acid solution of yttrium nitrate and a macrocyclic cavitand cucurbituryl. According to X-ray diffraction data, the crystal structure of the compound involves alternating layers of cucurbituryl molecules and eight-coordinate yttrium aqua complexes. The structure has a complex system of hydrogen bonds involving the oxygen atoms of cucurbituryl and water molecules and the nitrate anions and linking all structural elements of the crystal.     

Synthesis, structure, and characterization of a 1D monocopper substituted Dawson-type arsenotungstate (H2En)0.5[Cu(En)2]0.5{[Cu(En)2(H2O)]2[Cu(En)2] (α1-As2W17CuO61)} · 8H2O

A new 1D organic-inorganic hybrid monocopper substituted Dawson-type arsenotungstate (H₂En)_0.5[Cu(En)₂]_0.5{[Cu(En)₂(H₂O)]₂[Cu(En)₂](α₁-As₂W₁₇CuO₆₁)} · 8H₂O (I) has been hydrothermally synthesized by the reaction of Na₈[A-α-HAsW₉O₃₄] · 11H₂O, CuCl₂ · 2H₂O, YCl₃, with enthylenediamine (En) and characterized by elemental analyses, IR spectra, UV spectra, powder X-ray diffraction, thermogravimetric analysis, as well as single-crystal X-ray diffraction. Single-crystal structural analysis shows that I displays an interesting 1D chain constructed from [α₁-As₂W₁₇CuO₆₁]⁸⁻ subunits by means of common oxygen atoms and [Cu(En)₂]²⁺ bridges. It should be noted that the structural transformation of the trivacant Keggin polyoxoanion [A-α-AsW₉O₃₄]⁹⁻ to the monovacant Dawson [α-As₂W₁₇O₆₁]¹⁰⁻ polyoxoanion was observed. The TG curve of I exhibits three stages of weight loss.     

Crystal structure of calcium cis(N)-bis(iminodiacetato)chromate(III) nonahydrate Ca[Cr(Ida)2]2·9H2O

In the crystals of [Ca(H₂O)₅][Cr(Ida)₂]₂·4H₂O (triclinic symmetry, a = 10.1056(10) ?, b = 13.0077(11) ?, c = 13.1185(13) ?, α = 70.186(11)°, β = 81.248(11)°, γ = 78.996(11)°, Z = 2, space group P ) cyclic centrosymmetric tetramers are present. In them calcium ions are bonded to oxygen atoms of the carboxyl groups of two octahedral complex cis(N)-[Cr(Ida)₂]⁻ ions (Ida is the iminodiacetic acid anion). The O atoms of five water molecules complete the Ca atom environment to a distorted pentagonal bipyramid. Isolated [Cr(Ida)₂]⁻ ions of a similar structure neutralize the positive charge of tetramers. Original Russian Text Copyright ? 2009 by M. Zabel, V. I. Pavlovskii, and A. L. Poznyak __________ Translated from Zhurnal Strukturnoi Khimii, Vol. 50, No. 3, pp. 602–604, May–June, 2009.     

Crystal structure of [Pd(NH3)4]3[Ir(NO2)6]2·H2O

A single crystal of [Pd(NH₃)₄]₃[Ir(NO₂)₆]₂·H₂O double complex salt is studied by X-ray diffraction. Crystallographic characteristics are as follows: a = 21.0335(5) ?, b = 8.0592(2) ?, c = 21.3452(5) ?, β = 91.254(1)°, V = 3617.43(15) ?³, P2₁/c space group, Z = 4, d _x = 2.714 g/cm³. Single-layer pseudohexagonal packing of complex anions is determined along the [−1 0 1] direction in the structure. Complex cations and crystallization water molecules are located between the mentioned layers.     

Nine-coordinate dinuclear Na6[Gd 2III (Ttha)2] · 8H2O and mononuclear (H2En)3[GdIII(Ttha)]2 · 11H2O complexes: Synthesis and structural determination

The Na₆[Gd₂^III(Ttha)₂] · 8H₂O (I) (H₆Ttha = triethylenetetramine-N,N,N′,N″,N‴,N‴-hexaacetic acid) and (H₂En)₃[Gd^III(Ttha)]₂ · 11H₂O (II) (En = ethylenediamine) complexes were prepared with heat-refluxing and acidity-adjusting methods, respectively. Their composition and structures were determined by elemental analysis and single-crystal X-ray diffraction techniques. Complex I shapes a binuclear and nine-coordinated structure and crystallizes in the orthorhombic crystal system with space group Pccn. The central Gd³⁺ ion is coordinated with one Ttha ligand by three N atoms and four O atoms and with one adjacent Ttha ligand by two O atoms. The crystal data are as follows: a = 26.036(13) ?, b = 21.007(10) ?, c = 22.694(12) ?, V = 12412(11) ?³, Z = 8, c = 1.699 g/cm³, μ = 2.254 mm⁻¹, F(000) = 6368, R = 0.0602, and wR = 0.1146 for 3434 observed reflections with I ≥ 2σ(I). The GdN₃O₆ part in the [Gd₂^III(Ttha)₂]⁶⁻ complex anion forms a pseudo-tricapped trigonal prismatic geometry. Complex II is also nine-coordinate, but mononuclear and crystallizes in the monoclinic crystal system with space group P2₁/n. While the central Gd³⁺ ion is coordinated by four nitrogen atoms and five oxygen atoms from the same Ttha ligand. The crystal data are as follows: a = 17.7726(17) ?, b = 19.2942(17) ?, c = 20.6045(19) ?, β = 111.4600(10)°, V = 6575.6(10) ?³, Z = 8, c = 1.693 g/cm³, μ = 2.102 mm⁻¹, F(000) = 3428, R = 0.0333 and wR = 0.0827 for 14792 observed reflections with I ≥ 2σ(I). Otherwise, the GdN₄O₅ part in each [Gd^III(Ttha)]³⁻ complex anion adopts a pseudo-monocapped square antiprismatic polyhedron.     

Crystal and Molecular Structures of Barium cis(NO2)-trans(N)-Bis(glycinato)dinitrocobaltate(III) Hydrate [Ba(H2O)4][Co(Gly)2(NO2)2]2 · 1.43H2O

Crystals of [Ba(H₂O)₄][Co(Gly)₂(NO₂)₂]₂ · 1.43H₂O (a=8.1917(6) , b=8.4440(4) , c=19.444(1) , =98.189(9)°, Z=2, space group P2/n) contain infinite strips of alternating axially symmetric [Ba(H₂O)₄]²⁺ fragments and two dinitro-bis(glycinato)cobaltate(III) ions. In addition to four oxygen atoms of water molecules, the nearest environment of Ba includes six oxygen atoms of the carboxyl groups of four anions, two of which are also coordinated by the cobalt atoms (Ba-O, 2.77–3.01 ). The nitrite ions do not interact with the Ba²⁺ ions.__________Translated from Koordinatsionnaya Khimiya, Vol. 31, No. 5, 2005, pp. 329–332.Original Russian Text Copyright © 2005 by Zabel, Poznyak, Pawlowski.     

[Pb2(TNR)2(CHZ)2(H2O)2]·4H2O和[Cd(CHZ)2(TNR)(H2O)]快速热分解过程的研究

利用温度跃升傅立叶变换红外原位分析技术在0.1MPa氩气的条件下，对斯蒂酚酸碳酰肼铅和斯蒂酚酸碳酰肼镉的快速热分解过程进行了研究。研究结果表明，斯蒂酚酸碳酰肼铅的主要热分解气体为NH₃, H₂O和 HONO，而斯蒂酚酸碳酰肼镉的主要热分解气体为CO 和 NO，因此斯蒂酚酸碳酰肼镉不满足作为环境友好起爆药的使用要求。这两种化合物在快速热分解过程中均产生金属异氰酸盐、金属碳酸盐和金属氧化物。利用Real程序计算其燃烧温度可得斯蒂酚酸碳酰肼铅的燃烧温度要高于斯蒂酚酸碳酰肼镉，对其燃烧产物进行计算，发现HNCO不在燃烧产物之列，NO的含量也比实验得出的浓度要小。     

Synthesis and crystal structure of [Na2(μ-H2O)(H2O)CB[5]]Cl2 · 6H2O, [Na3(μ-H2O)4(H2O)4(CNPy@CB[6])]Cl3 · 8H2O, and [Rb2(μ-H2O)2(CNPy@CB[6])]Cl · 8H2O

The chain coordination polymers [Na₂(μ-H₂O)(H₂O)CB[5]]Cl₂ · 6H₂O (I), [Na₃(μ-H₂O)₄(H₂O)₄(CNPy@CB[6])]Cl₃ · 8H₂O (II), and [Rb₂(μ-H₂O)₂(CNPy@CB[6])]Cl₂ · 8H₂O (III) were prepared by heating (110°C) of a mixture of sodium or rubidium chloride, cucurbit[n]uril (CB[n], where n = 5, 6), 4-cyanopyridine, and water. According to X-ray diffraction data, binding of polynuclear cations with CB[n] in I–III occurs through coordination of the oxygen atoms of the cucurbit[n]uril portals to alkali metal atoms. Complexes I–III of the above composition isolated to the solid phase as supramolecular compounds with CB[n] were structurally characterized for the first time.     

Synthesis and structure of [Ni(dien)2]3[W4S4(CN)2]·20H2O and [Cu(dien)(Hdien)]2[W4S4(CN)12]·8H2O

[Ni(dien)₂]₃[W₄S₄(CN)₁₂]·20H₂O and [Cu(dien)(Hdien)]₂[W₄S₄(CN)₁₂]·8H₂O were obtained by evaporating water-ammonia solutions containing K₆[W₄S₄(CN)₁₂]·2H₂O·2CH₃OH, diethylene triamine, and NiCl₂·6H₂O or CuCl₂·6H₂O. The crystals of the complex compounds were obtained within 3 days. The complex compounds were characterized by IR spectroscopy and by XRD and elemental analysis. XRD data for the complex [Ni(dien)₂]₃[W₄S₄(CN)₁₂]·20H₂O are: triclinic system, , a = 14.671(2) Å, b = 16.448(3) Å, c = 19.814(3) Å, α = 67.841(3)°, β = 68.996(3)°, γ = 67.527(3)°, V = 3961.6(11) ų, Z = 2; for the complex [Cu(dien)(Hdien)]₂[W₄S₄(CN)₁₂]·8H₂O: monoclinic system, C2/c, a = 37.4290(1) Å, b = 17.7370(1) Å, c = 25.7370(2) Å, β = 105.3840(2)°, V = 16474.02(16) ų, Z = 12. Original Russian Text Copyright ? 2005 by I. V. Kalinina, D. G. Samsonenko, Z. A. Starikova, A. A. Korlyukov, J. Lipkowski, V. P. Fedin, and M. Yu. Antipin __________ Translated from Zhurnal Strukturnoi Khimii, Vol. 46, No. 1, pp. 139–148, January–February, 2005.     

Synthesis and Crystal Structure of [Zn(FcCOO)2(2,2′-bipy)(H2O)]2·H2O

A novel complex [Zn(FcCOO)2(2,2′-bipy)(H2O)]2·H2O (Fc = (η5-C5H5)Fe(η5-C5H4), 2,2′-bipy = 2,2′-bipyridine) has been synthesized and characterized by elemental analysis, IR and X-ray diffraction. It crystallizes in monoclinic system, space group P21/c with a = 6.8187(4), b = 21.7155(13), c = 19.7411(12) (A), α = 90, β = 97.7420(10), γ = 90°, C64H58Fe4Zn2N4O11, Mr = 1413.28, V = 2896.4(3) (A)3, Dc = 1.620 g/cm3, Z = 2, F(000) = 1444, μ(MoKα) = 1.857 mm-1, R = 0.0523 and wR = 0.0982 for 3219 observed reflections (I ＞ 2σ(I)). Structural analysis shows that the zinc atom is coordinated with three oxygen atoms from two ferrocenemonocarboxylates and one water molecule together with two nitrogen atoms from 2,2′-bipyridine, giving a distorted square-pyramidal coordination geometry. The complex molecules are linked to form an infinite one-dimensional chain by both intermolecular hydrogen bonds and π-π stacking interactions of the bipyridine rings.     

Crystal structures of barium bis(iminodiacetato)cobaltates(III): [Ba(H2O)6][Co(Ida)2]2 · H2O and Ba4(H2O)14][Co(Ida)2]5(ClO4)3 · 5.46H2O · 2CH3OH

The structures of the crystals of Ba₄[trans(N)-Co(Ida)₂]₃[cis-(N)-Co(Ida)₂]₂(ClO₄)₃ · 19.46H₂O · 2CH₃OH (I) and Ba[trans-(N)-Co(Ida)₂]₂ · 7H₂O (II) (H₂Ida is iminodiacetic acid) were determin by X-ray diffraction. The crystals of I containing two geometric isomers of the complex anions [Co(Ida)₂]⁻ were obtained by a slow cooling of a hot solution, which contained initially only the cis-isomer. One Ba atom in I interacts with the trans-complex and with two cis-complexes to give a three-dimensional framework in crystal I. The positive charge of the last framework is compensated by one more trans-complex and by the perchlorate ions, one of which acts as a bidentate ligand with respect to the Ba atom. The crystals of II are built of the chains with the alternating Ba atoms and the trans-(N)-[Co(Ida)₂]⁻ anions. The other anions of the same structure are each “suspended” to the Ba atoms of the chain. Original Russian Text ? M. Zabel, A.I. Poznyak, V.I. Pawlowskii, 2008, published in Koordinatsionnaya Khimiya, 2008, Vol. 34, No. 11, pp. 831–836.     

Synthesis and structures of nine-coordinate K[Dy(Edta)(H2O)3] · 3.5H2O, (NH4)3 [Dy(Ttha)] · 5H2O, and eight-coordinate NH4[Dy(Cydta)(H2O)2] · 4.5H2O complexes

The title complexes, K[Dy(Edta)(H₂O)₃] · 3.5 H₂O (I) (H₄Edta = ethylenediamine-N,N,N′,N′-tetraacetic acid), (NH₄)₃[Dy(Ttha)] · 5H₂O (II) (H₆Ttha = triethylenetetramine-N, N,N′,N″,N‴,N‴-hexaacetic acid), and NH₄[Dy(Cydta)(H₂O)₂] · 4.5H₂O (III) (H₄Cydta = trans-1,2-cyclohexanediamine-N,N,N′,N′-tetraacetic acid), were prepared, and their compositions and structures were determined by elemental analyses and single-crystal X-ray diffraction techniques, respectively. In complex I, the Dy³⁺ ion is nine-coordinated by an Edta ligand and three water molecules, yielding a pseudo-monocapped square antiprismatic conformation, and the complex crystallizes in the orthorhombic crystal system with space group Fdd2. The crystal data are as follows: a = 19.751(7), b = 35.573(12), c = 12.227(4) ?, V = 8591(5) ?³, Z = 16, space group Fdd2 ρ_c = 1.877 g/cm³, μ = 3.742 mm⁻¹, F(000) = 4800, R = 0.0259, and wR = 0.0616 for 3218 observed reflections with I ≥ 2σ(I). For complex II, the Dy³⁺ ion is nine-coordinated by a Ttha ligand, yielding a pseudo-monocapped square antiprismatic conformation, and the complex crystallizes in the monoclinic crystal system with space group P2₁/c. In addition, there is a free non-coordinate carboxyl group (-CH₂COO⁻) in the [Dy(Ttha)]³⁻ complex anion. The crystal data are as follows: a = 10.353(3), b = 12.746(4), c = 23.141(7) ?, β = 91.005(5)°, V = 3053.2(15) ?³, Z = 4, space group P2₁/c ρ_c = 1.730 g/cm³, μ = 2.532 mm⁻¹, F(000) = 1620, R = 0.0332 and wR = 0.0924 for 5390 observed reflections with I ≥ 2σ(I). For complex III, the Dy³⁺ ion is eight-coordinated by a ligand Cydta and two water molecules, yielding a distorted square antiprismatic conformation, and the complex crystallizes in the triclinic system with space group P . The crystal data are as follows: a = 8.604(3), b = 10.012(4), c = 14.369(6) ?, α = 88.330(6)°, β = 75.363(6)°, γ = 88.285(6)°, space group P V = 1196.9(8) ?³, Z = 2, ρ_c = 1.776 g/cm³, μ = 3.194 mm⁻¹, F(000) = 644, R = 0.0445 and wR = 0.1041 for 3931 observed reflections with I ≥ 2σ(I). The article is published in the original.     

Synthesis, thermogravimetric analysis, IR spectrum, and the crystal structure of sodium hexatunstomanganate [Na2(H2O)10][Na(H2O)3]2[MnW6O18(OH)6] · 6H2O

The complex [Na₂(H₂O)₁₀][Na(H₂O)₃]₂[MnW₆O₁₈(OH)₆] · 6H₂O was synthesized and studied by mass spectrometry, thermogravimetry, IR spectroscopy, X-ray diffraction. The crystals are monoclinic, space group P2₁/n, a = 11.698(2), b = 11.670(2), c = 14.652(3) ?, β = 102.52(3)°, V = 1952.7(7) ?³, ρ(calcd.)= 3.45 g/cm³, Z = 2.     

Synthesis and crystal structure of Na4[Er2(EDTA)2(μ2-C2O4)] · 8H2O (where EDTA stands for ethylenediamine-N,N′-tetraacetate)

Synthesis was carried out, and structure solved for the new dinuclear erbium(III) complex having a composition of Na₄[Er₂(EDTA)₂(C₂O₄)] · 8H₂O (where EDTA stands for ethylenediamine-N,N′-tetraacetate). The compound was characterized by IR and UV spectroscopy, mass spectrometry, and X-ray crystallography. In the structure of the compound, erbium(III) has C.N. 8 and a coordination polyhedron shaped as a square antiprism. The EDTA and oxalate ions manifest their characteristic coordination modes: N,O-chelate hexadentate and bridge-cyclic tetradentate, respectively.     

Crystal structure of metal-organic coordination polymers [Cu(bpy)2(H2O)2](NO3)2·4.5C2H5OH and [Cu2(bpy)(H2O)(L-pha)2](NO3)2·H2O

Two metal-organic coordination polymers [Cu(bpy)₂(H₂O)₂](NO₃)₂·4.5C₂H₅OH (1) and [Cu₂(bpy)(H₂O)(L-pha) ₂](NO₃)₂·H₂O (2) (L-Hpha = L-phenylalanine, bpy = 4,4′-bipyridyl) are prepared by slow evaporation of an aqueous alcoholic solution of copper nitrate, L-phenylalanine, and 4,4′-bipyridyl. The structure and composition of the obtained compounds are determined by single crystal XRD. The framework of compound 1 is positively charged and forms two types of intersecting channels. Compound 2 is a homochiral metal-organic coordination polymer whose structure contains L-phenylalanine anions.     

trans-dinitro- and trans-dinitratoruthenium complexes [RuNO(NH3)2(NO2)2(OH)] and [RuNO(NH3)2(H2O)(NO3)2]NO3·H2O

Methods for the synthesis of trans-diammino complexes [RuNO(NH₃)₂(NO₂)₂(OH)] (I) and [RuNO(NH₃)₂(H₂O)(NO₃)₂](NO₃)·H₂O (II) are suggested. The compounds were studied by IR spectroscopy and X-ray phase and X-ray structural analyses. Crystal data: space group P-1; a = 6.2328(2) ?, b = 11.0488(3) ?, c = 11.0981(4) ?, α = 71.942(1)°, β = 83.291(1)°, γ = 86.877(1)° (I); space group P2₁; a = 6.6290(2) ?, b = 13.4389(5) ?, c = 7.0180(2) ?, β 114.281(1)° (II). Complex II readily lost some part of crystal water on storage in open air. Original Russian Text Copyright ? 2009 by M. A. Il’in, E. V. Kabin, V. A. Emel’yanov, I. A. Baidina, and V. A. Vorob’yov __________ Translated from Zhurnal Strukturnoi Khimii, Vol. 50, No. 2, pp. 341–348, March–April, 2009.     

Structure of tetra(3,5-dinitrobenzoate) bis(Piperidine) hexaaquanickel(II)—[Ni(OH2)6](PipH)2(3,5-DNB)4·2H2O dihydrate

It is found that M(AmH)₂(3,5-DNB)₄·8H₂O compounds (where M(II) = Co, Ni; AmH is piperidine PipH = (C₅H₁₀NH₂)⁺ or diethylamine DaH = (C₄H₁₀NH₂)⁺ cations; 3,5-DNB = (C₇H₃N₂O₆)⁻ is the dinitrobenzoic acid anion) are isotypic. The structure of the Ni(PipH)₂(3,5-DNB)₄·8H₂O single crystal is studied. The crystals have a monoclinic system, P2₁/n space group, Z = 2, a = 6.7694(3) ?, b = 16.0746(6) ?, c = 23.1250(9) ?, β = 97.794(1)°, V = 2493.1(2) ?³, T = 153 K. The final value R(F) = 0.0407 was obtained for 8191 independent reflections with I> 2σ(I). The structural units of the compound studied are as follows: [Ni(OH₂)₆]²⁺ complex hexaaquacation, two (PipH)⁺ cations, four (3,5-DNB)⁻ anions, and two molecules of water of crystallization with the structural formula [Ni(OH₂)₆](PipH)₂(3,5-DNB)₄·2H₂O. Similar compounds of Ni(II) and Co(II) are isostructural.