Synthesis and crystal structure of catena-μ-chloro-bis(acetonitrile)copper(I) [(H3CCN)2CuCl]∞

The new crystalline compound of catena--chloro-bis(acetonitrile)copper(I) [(H₃CCN)₂ CuCl] has been synthesized and structurally characterized by X-ray crystallography. The compound is an infinite polymeric chain in which chlorides bridge the coppers. Copper exhibits tetrahedral coordination geometry with two acetonitrile molecules acting as coordinating ligands. The compound crystallizes in the orthorhombic Pbcm space group with a = 12.585(3) Å, b = 7.496(2) Å, and c = 7.275(2) Å.     

Crystal structure of [{MoBr2(O){OPH(OPr i )2}2}2(μ-O)]

[{MoBr₂(O){OPH(OPr ⁱ )₂}₂}₂(μ-O)] (1) crystallizes in the monoclinic space group P2₁/n, with a = 13.063(17) Å, b = 11.818(14) Å, c = 15.889(17) Å, β = 90.30(1)°, Z = 2. The dimeric structure contains a bridging oxygen atom at a crystallographic center of symmetry. Each octahedral molybdenum center has trans-bromide ligands, and two cis-OPH(OPr ⁱ )₂ units, with a terminal oxygen atom trans to one of the OPH(OPr ⁱ )₂ units.     

配位聚合物{[Co3(TCOPM)2(H2O)2]·17H2O}n的合成和结构

采用三(对-苯甲酸)甲烷(H3TCOPM)为配体,以Co为中心离子采用自组装的方法合成了配位聚合物{[Co3(TCOPM)2(H2O)2]·17H2O}n,利用单晶衍射仪,红外光谱,TG和元素分析对其进行了晶体结构的解析和表征.它属于单斜晶系,C2/c空间群,晶胞参数分别为a=2.9675(13) nm,b =1.3548(5) nm,c=1.8659 (5) nm,α=90.00°,β=124.61(2)°,γ=90.00°,V=6.174(4) nm3,Mr=959.47,Z=4,Dc=1.187 g/cm3,μ =0.860 mm-1,F(000)=2268.0.结果表明,配位聚合物中H3TCOPM的三个羧酸全部和Co配位,形成三维结构,展现了一个具有tfd连接拓扑网络结构,其孔隙率为47.6;.     

Crystal and molecular structure of di-μ-chlorobis[2-[[[(2-hydroxy-1-naphthyl)methyl]-imino]ethanolato]N,O,O′]di-copper(II) dihydrate

The crystal structure of the title compound has been determined from three-dimensional, single crystal X-ray diffraction data. [Cu₂Cl₂(C₁₃H₁₂NO₂)₂]·2H₂O crystallizes in the orthorhombic space group P2₁2₁2₁ with lattice constants,a=11.866(2),b=13.555(3),c=17.380(3) Å. Final full-matrix least-squares refinement of 3735 unique reflections yieldedR=0.054. The structure consists of dimeric C₂₆H₂₄Cl₂Cu₂N₂O₄ molecules and water molecules connected with the dimeric molecules by a hydrogen bond system. Both of the copper(II) centers are five-coordinated by twotrans oxygen atoms and one nitrogen atom from one ligand molecule and two chloride ions. The geometry at each copper(II) center is best described as distorted tetragonal pyramidal. The apical Cu1–Cl2 and Cu2–C11 distances are 2.747(2) and 2.938(3)Å, respectively. The Cu...Cu separation is 3.496(1)Å. The comparison with previously reported crystal structure of [Cu₂Cl₂ (C₁₃H₁₂NO₂)₂]·1/2H₂O is given.     

Seven-coordinated chelate [Cd(SCZ)3·H2O](HTNR)2(H2O)2: Synthesis,crystal structure and energetic properties

To deepen the study on heptacoordinate transition metal coordination complexes, a novel seven-coordinated coordination compound [Cd(SCZ)₃·H₂O](HTNR)₂(H₂O)₂ (1, SCZ = semicarbazide, H₂TNR = styphnic acid) was synthesized and characterized by elemental analysis and FTIR spectroscopy. Single-crystal X-ray diffraction analysis revealed that 1 crystallizes in the triclinic space group P-1. The thermal decomposition mechanism of 1 was studied by differential scanning calorimetry (DSC). The non-isothermal kinetics parameters were calculated by the Kissinger's method and Ozawa-Doyle's method, respectively. Sensitivity tests revealed that 1 is insensitive to mechanical stimuli. The heat of combustion was measured by oxygen bomb calorimetry and the enthalpy of formation was calculated.     

The crystal and molecular structure of 14-β-N-pentylaminomorphinone,C22H28N2O3

The crystal and molecular structure of 14--N-pentylaminomorphinone (14--N-PAM), C₂₂H₂₈N₂O₃, has been determined by analysis of single crystal X-ray diffraction data. The compound crystallized at room temperature in the orthorhombic system, space group P2₁2₁2₁ witha=12.4535(8),b=13.7855(8),c=11.710(1) Å,V _c =2010.3(2) ų,Z=4,D _x =1.22 gm/cm³,(Cu K)=6.58 cm^–1, andF(000)=792. The final refinement yieldedR=0.051,R _w =0.059 for 328 variables with 1133 unique observed reflections. The absolute configuration is established via the synthesis from thebaine by the noninvolvement of certain asymmetric centers. The molecule is found to have as its central structure a T shape similar to that found in morphine and codeine. The distinctive feature of the molecule is the 14--N-pentylamino lipophilic side chain. Molecular modeling studies on the alkylamino chain result in the identification of clusters of conformations based on energy and dihedral angle criteria. Selected conformations are compared to 19-propylthevinol (etorphine), another potent analgesic which contains a lipophilic hydroxyalkyl substituent at C19. The enhanced analgesic activity of 14--N-pentylaminomorphinone is postulated to arise from an overall morphine-like contact with the receptor augmented by the interaction of the aliphatic chain with a lipophilic receptor pocket.     

Crystal structure of tetrabutylammonium nitroprusside dihydrate, [(C4H9)4N]2[Fe(CN)5NO]·2H2O, and vibrational spectra of ground and metastable excited states of the dihydrate and the anhydrate

The crystal structure of tetrabutylammonium nitroprusside dihydrate (TBANPDH, [(C₄H₉)₄N]₂[Fe(CN)₅NO]·2H₂O) was determined by single crystal X-ray diffraction (XRD) and the compound was also studied, as well as the anhydrous salt (TBANP), by room and low temperature Fourier Transform Infra-Red (FTIR) and room temperature Fourier Transform Near Infra-Red Raman (FTNIRR) spectroscopies. In addition to the ground states (GS), the metastable excited states (MSI and MSII) generated by laser excitation (488 nm) at low temperature were IR studied, both of the dihydrate and the anhydrate. TBANPDH crystallizes in the trigonal space group P3₂21, D ⁶ ₃, with a = b = 13.777(2), c = 22.039(2) Å, and Z = 3. The structure was solved employing 1273 independent XR reflections, with I > 2(I), by Patterson and Fourier methods and refined by full-matrix least-squares to R1 = 0.054.     

Crystal structure of aqua[S-prolinato-N-monoacetato)copper(II) dihydrate [Cu(Proma)H2O] ⋅ 2H2O

The crystal structure of [Cu(C₇H₉NO₄)H₂O] ? 2H₂O is determined by X-ray diffraction (λMo, R = 0.0316 for 857 reflections). The crystals are tetragonal, a = 8.219(1) Å, c = 17.449(3) Å, Z = 4, ρ_calcd = 1.627 g cm^?3, and space group P4₃. The coordination polyhedron of the Cu atom is a tetragonal pyramid with the O atom of the acetate arm of the prolinatomonoacetate ion (Proma) in the apical position [Cu-O 2.312(6) Å]. The O atom of the water molecule and the N and O atoms of the prolinate group of the Proma ligand lie in the basal plane. The Cu-N bond length is 2.044(6) Å, and the Cu-O bond lengths are 1.932(7) and 1.927(6) Å. The O atom of the acetate arm of the neighboring Proma ion completes the basal plane [Cu-O 1.951(6) Å], thus linking the copper complexes into infinite chains.     

2D配位聚合物{[Eu(pdc)(ox)0.5(H2O)4]·2H2O}n的结构和荧光性质

用氯化铕和2,4-吡啶二甲酸在水热条件下反应合成了一个二维铕稀土配位聚合物{[Eu (pdc) (ox)05(H2O)4]·2H2O}n(1)(H2pdc=2,4-吡啶二甲酸;ox=草酸根阴离子),草酸根离子由部分2,4-吡啶二甲酸分解产生.X-射线单晶衍射分析表明,该配位聚合物属单斜晶系,P121/c1 (No.14)空间群,晶胞参数为a=1.53047(15) nm,b=1.10973(9) nm,c =0.85494(15) nm,β=102.81(1)°,α=y =90°.Eu3+为九配位,除了与一个pdc阴离子配体和一个ox阴离子配体螫合配位外,还与四个水分子配位.pdc阴离子通过2-位羧基以μ2-桥联方式连接两个Eu3+,吡啶环上的氮原子与其中一个Eu3+配位,4-位羧基没有参与配位.草酸根阴离子以螯合方式连接两个Eu3+.配体pdc和ox与Eu3+通过配位键连接形成了少见的2D之字形平面,该配合物在紫外光的激发下显示鲜艳的红色荧光,表明该配位聚合物具有良好的荧光性质,热重分析表明该配位聚合物具有较好的热稳定性.     

Synthesis of [Mn(O2CCH2CH2CO2)(2,2′-bipyridyl) (H2O)2]n·H2O

The title compound exists as a 1D coordination polymer consisting of succinate anions, manganese cations and 2,2-bipyridyl molecules. Twelve water molecules are present in the unit cell and are part of a hydrogen bonding system. Some of these waters are binding to manganese cations while others are only participating in hydrogen bonding. The structure has a monoclinic space group P2₁/c with a = 8.2750(3) Å, b = 11.5104(3) Å and c = 16.9113(6) Å, = 95.2727(16); V = 1603.96(9) ų and Z = 4.     

Crystal and molecular structure of [Cu2(3,5-dihydroxybenzoate)4 (acetonitrile)2] ⋅ 8H2O

The crystal and molecular structure of the title compound, [Cu₂(3,5-dihydroxybenzoate)₄ (acetonitrile)₂] 8H₂O 1, is reported. Crystal data for 1: tetragonal, space group I 4/m, a = 11.720(2) Å, c = 15.304(3) Å, V = 2102.4(6), and D _c = 1.53 g/cm³, for Z = 2. The metal and organic components crystallize to form a Cu paddle-wheel complex, of idealized D_4h symmetry, that assembles in the solid-state, along with eight equivalents of water, to form a 3D hydrogen-bonded network held together by O–H O hydrogens bonds. The metal complexes pack to form a 2D layered structure.     

Synthesis and X-ray structure of [(μ-H)Os3(CO)10(μ-η2-N=CCH=CHCH=CC2H5)]

The reaction of [Os₃(CO)₁₀(MeCN)₂] with 2-ethylpyridine at ambient temperature leads to the isolation of the cluster [(-H)Os₃(CO)₁₀(-²-N=CCH=CHCH=CC₂H₅)][3 (65% yield) which has been structurally characterized by crystallographic methods. The compound crystallizes in the triclinic space group with a = 9.334(2), b = 9.918(2), c = 11.767(1) Å, = 92.13(2), = 99.93(1), = 99.88(2)°, V = 1054.7(3) ų and Z = 2. The same edge of the osmium triangle in the cluster is bridged by both the hydrido and the heterocyclic ligands, the latter through the nitrogen and the carbon atoms of the C=N bond.     

The crystal structure analysis of iron nitroprusside,Fe[Fe(CN)5NO]·3H2O

The crystal structure of iron(II) pentacyanonitrosylferrate trihydrate has been determined from three dimensional, single-crystal X-ray diffraction data. Fe[Fe(CN)₅NO]·3H₂O crystallizes in the monoclinic space group P2₁/n with lattice constants,a=7.205(1),b=14.641(2),c=10.680(1) Å,=91.14(1)° andZ=4,D _m =1.89(1) g cm^–3 andD _x =1.92 g cm^–3. Final full-matrix least-squares refinement of 1691 unique reflections yieldedR=0.024 andR _w =0.028. Both iron atomic centers have distorted octahedral symmetries. The cation iron center is coordinated by five cyanide ligands and one water molecule, while the second iron center is coordinated by five cyanide ligands and one nitrosyl group. Cyanide bridging links the metal centers. Two uncoordinated water molecules, O(2) and O(3), are hydrogen bonded to the coordinated water molecule, O(1), and occupy channels in the crystal lattice. Important mean bond distances for iron nitroprusside are: Fe(cation)-N=2.159(17), Fe-C=1.936(4) and C=N=1.144(6) Å. Other notable bond lengths include: Fe-O(1)=2.152(2), Fe-NO=1.669(2) and NO=1.131(3) Å. The distances between the coordinated water molecule and two uncoordinated water molecules are 2.855(3) and 2.740(3) Å.     

{[La(phen-dione)2(H2dhtp)0.5(H2O)]·H2O}n配合物的合成、晶体结构及荧光性质

采用低温水热法合成了一个新的镧(Ⅲ)配位聚合物{[La(phen-dione)2(H2dhtp)0.5(H2O)]·H2O}n(phen-dione＝1,10-邻菲啰啉-5,6-二酮,H2dhtp＝2,5-二羟基对苯二甲酸酯).单晶衍射分析结果表明,该配合物属三斜晶系,P-1空间群,晶胞参数为a＝9.4600(19)nm,b ＝11.810(2)nm,c ＝12.280(3)nm,α＝93.34(3)°,β＝106.74(3)°,γ＝103.21(3)°,V＝1267.7(5)nm3,Dc ＝1.806 g/cm3,Z＝2,μ＝1.752mm-1,F(000)＝678.用X-射线单晶衍射、元素分析、IR、TG和荧光光谱对配合物进行了表征.测量晶体的荧光光谱特性发现,该配合物在488 nm 和532nm有较强的荧光发射峰.     

Synthesis, crystal structure, and thermal analyses of triaqua-(1,10-phenanthroline-N,N′) succinatomanganese(II) dihydrate, [Mn(H2O)3(phen)(C4H4O4)]·2H2O

[Mn(H₂O)₃(phen)(C₄H₄O₄)]·2H₂O was obtained by reaction of freshly prepared MnCO₃, phen and succinic acid in CH₃OH/H₂O (1:1 v/v), and its crystal structure has been determined by single crystal X-ray diffraction methods. The title mixed ligand complex crystallizes in the triclinic space group with cell dimensions a = 7.590(1) Å, b = 9.324(1) Å, c = 13.917(1) Å, = 85.64(1)°, = 74.56(1)°, = 77.10(1)°, and D _calc = 1.584 g/cm³ for Z = 2. The crystal structure consists of the [Mn(H₂O)₃(phen)(C₄H₄O₄)] complex molecules and lattice H₂O molecules. The Mn atoms are each octahedrally coordinated by two N atoms of one phen ligand and four O atoms of three H₂O molecules and one succinato ligand with d(Mn—N) = 2.271 and 2.299 Å, and d(Mn—O) = 2.133–2.239 Å. Through intermolecular hydrogen bondings, the complex molecules are interlinked to form 2D layers, which are assembled by – stacking interactions into 3D framework with tunnels occupied by the lattice H₂O molecules. Thermal analyses showed that the title compound decomposes in two steps over the range 25–600°C upon heating in flowing Ar.     

Synthesis and crystal structure of [(PhenH)(PhenH2)][BiCl6]·2H2O with different o-phenanthroline protonations

The reaction between bismuthate oxide and phen (1,10-phenanthroline) in acid medium led to the isolation of the unusual [(PhenH)(PhenH₂)][BiCl₆]·2H₂O derivative, which has been characterized by X-ray analysis and IR spectroscopy. The compound crystallizes in the triclinic space group with a = 8.313(2), b = 9.349(2), c = 9.807(3) Å, = 86.39(3), = 110.27(3) and = 106.48(3)°. The crystal structure is made of [BiCl₆]^3– anions and [(PhenH)(PhenH₂)]³⁺ cations. A network of hydrogen bond interactions involving the two clathrated water molecules, the phenanthroline moiety and the chlorines characterizes the entire structure.     

Refined crystal structure of lovozerite Na2CaZr[Si6O12(OH,O)6] · H2O

The structure of Na,Ca,Zr-silicate lovozerite, Na₂CaZr[Si₆O₁₂(OH,O)₆] · H₂O, from the Khibiny alkaline massif (the Kola Peninsula) was refined by single-crystal X-ray diffraction analysis (Syntex $P\bar 1$ diffractometer, λMoK _α radiation, 2θ/θ scanning technique). The refinement (R _hkl = 0.077, 1531 independent reflections; anisotropic thermal parameters) confirmed the trigonal system proposed for the mineral earlier (sp. gr. R3; a = 10.18(1) Å, c = 13.13(2) Å, Z = 3) and revealed the presence of two additional positions (C and B) statistically occupied by Ca and Na atoms (and partly by Mn) and H₂O molecules, respectively.     

Crystal structure of aminoguanidinium hexahydro-closo-hexaborate dihydrate, (CN4H7)2B6H6 · 2H2O

The (HAgu)₂B₆H₆ · 2H₂O compound was synthesized and its crystal structure was determined [R = 0.0385 for 2018 reflections with I > 2σ(I)]. The structure consists of HAgu ⁺ cations, centrosymmetric B₆H ₆ ^2? anions, and water molecules. The anions have an almost regular octahedral structure. The bond lengths and angles lie within the following narrow ranges: B-B, 1.715–1.726(2) Å; B-H, 1.08–1.14(2) Å; B-B-B, 59.72°–60.29(9)° and 89.63°–90.20(11)°; and B-B-H, 133.2°–137.0(9)°. The HAgu ⁺ cations and water molecules are involved in the O-H?O, N-H?O, and N-N?N hydrogen bonds and participate in numerous (N, O)-H?H-B specific interactions with the B₆H ₆ ^2? anions, which results in splitting and high-frequency shift of the band of B-H stretching vibrations in the IR spectrum.     

Synthesis and crystal structure of [Co(phen)(H2O)4](SO4)⋅2(H2O)

The title complex, [Co(phen)(H₂O)₄](SO₄)2(H₂O) (phen = 1,10-phenanthroline) was prepared in aqua tert-butylperoxohydrogen solution. X-ray single crystal structure determination reveals that the complex consists of a phenanthrolinatocobalt(II)tetrahydrate dication, two uncoordinated water molecules and a sulfate anion. It crystallizes in the orthorhombic space group Pbca with a = 8.856(1), b = 18.318(3), c =21.918(5) Å, V = 3555.6(11) ų. The coordination geometry at each cobalt(II) atom is a slightly distorted octahedron.     

Synthesis and crystal structure of [Ni(H2O)6](C19H17O9S)2·2H2O

A water soluble flavonoid sulfate, [Ni(H₂O)₆](C₁₉H₁₇O₉S)₂·2H₂O was synthesized and its structure was determined by single-crystal X-ray diffraction analysis. The crystal of it belongs to triclinic crystal system, space group P–1. The results show that the title compound consists of [Ni(H₂O)₆]²⁺, C₁₉H₁₇O₆SO₃ ⁻ and H₂O. Ni(II) is located on the symmetry center and octahedrally coordinated by six water molecules. A variety of hydrogen bonds among [Ni(H₂O)₆]²⁺, C₁₉H₁₇O₆SO₃ ⁻ and the lattice water molecules build a hydrophilic region. Aromatic π–π stacking interactions assemble isoflavone skeletons into a column and the columns form a hydrophobic region of the title compound. The sulfo-groups bridge the hydrophilic regions and the hydrophobic regions as well as the inorganic components and organic components. Hydrogen bonds, stacking interactions and the electrostatic interactions between cation [Ni(H₂O)₆]²⁺ and anion sulfonate C₁₉H₁₇O₆SO₃ ⁻ lead the moieties to a three-dimensional structure.