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1.
《Journal of Coordination Chemistry》2012,65(1):118-129
A new procedure developed for the synthesis and crystallization of various zinc(II) fumarate hydrate coordination polymers is described. In the first step, anhydrous Zn(II) fumarate, [Zn(C4H2O4)] (1), is synthesized from Zn(II) acetate and fumaric acid in methanol. Subsequently, this product is used as a starting material for growing small crystals of bis–aqua Zn(II) fumarate, [Zn(H2O)2(C4H2O4)] (2), triaqua Zn(II) fumarate monohydrate, [Zn(H2O)3(C4H2O4)]·H2O (3), tetraaqua Zn(II) fumarate, [Zn(H2O)4(C4H2O4)] (4), and tetraaqua Zn(II) fumarate monohydrate, [Zn(H2O)4(C4H2O4)]·H2O (5). All structures were determined or redetermined by X-ray structure analyses. The hitherto unknown compound 3 exhibits a zig-zag chain structure with five-coordinate Zn(II) ions. 相似文献
2.
Michael Gorol Nadia C. Msch‐Zanetti Mathias Noltemeyer Herbert W. Roesky 《无机化学与普通化学杂志》2000,626(11):2318-2324
Reaction of [M(NH3)6]Cl3 (M = Co, Rh, Ir) and [Ir(NH3)5(OH2)]Cl3 with (NH4)2C2O4 · H2O in aqueous solution resulted in the isolation of [M(NH3)6]2(C2O4)3 · 4 H2O and [Ir(NH3)5(OH2)]2(C2O4)3 · 4 H2O, respectively. The complexes have been characterized by X‐ray crystallography, IR and UV/VIS spectroscopy. The isomorphous compounds crystallize in the orthorhombic space group Pnnm (No. 58). Four molecules of crystal water are involved in an extended three‐dimensional hydrogen bonding network. The librational modes of the lattice water around 600 cm–1 allow the characterization of [Ir(NH3)6]2(C2O4)3 · 4 H2O and [Ir(NH3)5(OH2)]2(C2O4)3 · 4 H2O, respectively, by IR spectroscopy. The band around 600 cm–1 shows a significant frequency shift in the IR spectra of the hexaammine and aquapentaammine complex of iridium(III) and, by that, a distinction is possible. 相似文献
3.
New Osooxalatocomplexes of Molybdenum (VI) The preparation of the compounds Cs2[Mo2O5F2(C2O4)] · H2O and Cs2[Mo2O4Cl4(C2O4)] · 2 H2O is reported. The structure of the complex anions, which are containing quadridentated oxalate ligands, is derived from their vibration spectra. The compounds [NR4]2[Mo2O4F4(C2O4)] with R = CH3 and C2H5 are examined for comparison. 相似文献
4.
Tomoka Yamaguchi Yukinari Sunatsuki Hiroyuki Ishida 《Acta Crystallographica. Section C, Structural Chemistry》2008,64(4):m156-m160
In the crystal structures of both title compounds, [1,3‐bis(2‐hydroxybenzylidene)‐2‐methyl‐2‐(2‐oxidobenzylideneaminomethyl)propane‐1,3‐diamine]nickel(II) [2‐(2‐hydroxybenzylideneaminomethyl)‐2‐methyl‐1,3‐bis(2‐oxidobenzylidene)propane‐1,3‐diamine]nickel(II) chloride methanol disolvate, [Ni(C26H25.5N3O3)]2Cl·2CH4O, and [1,3‐bis(2‐hydroxybenzylidene)‐2‐methyl‐2‐(2‐oxidobenzylideneaminomethyl)propane‐1,3‐diamine]zinc(II) perchlorate [2‐(2‐hydroxybenzylideneaminomethyl)‐2‐methyl‐1,3‐bis(2‐oxidobenzylidene)propane‐1,3‐diamine]zinc(II) methanol trisolvate, [Zn(C26H25N3O3)]ClO4·[Zn(C26H26N3O3)]·3CH4O, the 3d metal ion is in an approximately octahedral environment composed of three facially coordinated imine N atoms and three phenol O atoms. The two mononuclear units are linked by three phenol–phenolate O—H...O hydrogen bonds to form a dimeric structure. In the Ni compound, the asymmetric unit consists of one mononuclear unit, one‐half of a chloride anion and a methanol solvent molecule. In the O—H...O hydrogen bonds, two H atoms are located near the centre of O...O and one H atom is disordered over two positions. The NiII compound is thus formulated as [Ni(H1.5L)]2Cl·2CH3OH [H3L is 1,3‐bis(2‐hydroxybenzylidene)‐2‐(2‐hydroxybenzylideneaminomethyl)‐2‐methylpropane‐1,3‐diamine]. In the analogous ZnII compound, the asymmetric unit consists of two crystallographically independent mononuclear units, one perchlorate anion and three methanol solvent molecules. The mode of hydrogen bonding connecting the two mononuclear units is slightly different, and the formula can be written as [Zn(H2L)]ClO4·[Zn(HL)]·3CH3OH. In both compounds, each mononuclear unit is chiral with either a Δ or a Λ configuration because of the screw coordination arrangement of the achiral tripodal ligand around the 3d metal ion. In the dimeric structure, molecules with Δ–Δ and Λ–Λ pairs co‐exist in the crystal structure to form a racemic crystal. A notable difference is observed between the M—O(phenol) and M—O(phenolate) bond lengths, the former being longer than the latter. In addition, as the ionic radius of the metal ion decreases, the M—O and M—N bond distances decrease. 相似文献
5.
The crystal structure of Ca[Cr(Edda)(C2O4)]2·5H2O and Ba[Cr(Edda)(C2O4)]2·5H2O (H2Edda — ethylenediamine-N,N′-diacetic acid) was determined by X-ray diffraction analysis. The nearest environment of alkaline earth ions consists of the oxygen atoms of the neighboring [Cr(Edda)(C2O4)]? complex ions (five for Ca and four for Ba) and the water molecules that complete the coordination number to eight. Two atoms and two complex ions are linked into a ring; each Ca atom in the ring is bonded by the oxalate ion bridge to another anion. This results in a centrosymmetric hexanuclear supramolecular assembly. The atoms and the complex anions alternate to form an infinite chain, in which each Ba atom is additionally linked via the oxalate ion bridge with one anion. 相似文献
6.
Two three-dimensional supramolecular water architectures, [Zn(phen)3]2·[Zn(C10H16O4)·(H2O)3]·(C10H16O4)2·20H2O (1) and [Co(phen)3]2·[Co(H2O)6]·(C10H16O4)3·30H2O (2) [phen = 1,10-Phenanthroline, C10H16O4 = sebacic dianion], have been synthesized and characterized by IR, elemental analysis, thermogravimetric analysis, and single-crystal X-ray diffractions. The two structures both contain extensive hydrogen bonding between water molecules as well as between water molecules and sebacic anions. The water molecules and sebacic acid O atoms assembled 2D supramolecular corrugated sheets with different morphology in the two complexes. 相似文献
7.
Gerrit G. Herman Werner Lippens Andr M. Goeminne Mathieu Steenland Norbert M. Blaton 《Acta Crystallographica. Section C, Structural Chemistry》2003,59(7):m294-m298
The crystal structures of (2,6‐dioxo‐1,4,7,11,14‐pentaazacycloheptadecanato)copper(II) tetrahydrate, [Cu(C12H23N5O2)]·4H2O, (I), (3,16‐dioxo‐1‐oxa‐4,8,11,15‐tetraazacycloheptadecanato)copper(II) pentahydrate, [Cu(C12H22N4O3)]·5H2O, (II), and (3,16‐dioxo‐1‐thia‐4,8,11,15‐tetraazacycloheptadecanato)copper(II) trihydrate, [Cu(C12H22N4O2S)]·3H2O, (III), are reported. The coordination geometry in each case is approximately square pyramidal with two amine groups and two deprotonated amide groups in the basal plane. The apical position is occupied by an amine group, an ether O atom or a thio S atom. Trigonal distortion increases in the sequence S < O < N as apical donor. The relation between the distortion in the basal plane of the complexes and the maxima in their electronic spectra is discussed. 相似文献
8.
Xin‐Yi Cao Jian Zhang Yao Kang Jian‐Kai Cheng Zhao‐Ji Li Xiao‐Qin Wang Yi‐Hang Wen Yuan‐Gen Yao 《Acta Crystallographica. Section C, Structural Chemistry》2004,60(7):m350-m352
In the title compound, {[Zn(C8H4O5)(C12H8N2)]·H2O}n or {[Zn(OH‐BDC)(phen)]·H2O}n (where OH‐H2BDC is 5‐hydroxyisophthalic acid and phen is 1,10‐phenanthroline), the Zn atoms are coordinated by two N atoms from the phen ligands and by four O atoms from hydroxyisophthalate ligands in a highly distorted octahedral geometry, with Zn—O distances in the range 2.042 (4)–2.085 (5) Å and Zn—N distances of 2.133 (5) and 2.137 (5) Å. The {[Zn(OH‐BDC)(phen)]·H2O}n infinite zigzag polymer forms a helical chain of [Zn2(OH‐BDC)2]n units. Face‐to‐face π–π interactions (3.60–3.75 Å) occur between two phen rings belonging to the same helical chain. Consolidation of the packing structure is achieved by O—H⋯O hydrogen‐bonding interactions between the carboxylate O atoms, the hydroxyl group and the water molecule, forming two‐dimensional sheets. 相似文献
9.
N. M. Samus’ A. P. Gulya V. I. Tsapkov Yu. M. Chumakov T. Roshu 《Russian Journal of General Chemistry》2006,76(7):1100-1105
Hydrates of 3-phenylpropenal thiosemicarbazone (HL·H2O) and semicarbazone (HL′·H2O) react in methanol with cobalt, nickel, copper, and zinc chlorides, nitrates, and acetates to form coordination compounds MX2·2HL·nSolv [M = Co, Ni, Cu, Zn; X = Cl, NO3; HL = C6H5CH=CH-CH=N-NHC(O)NH2; n = 0–3; Solv = H2O, CH3OH], CuX2·HL·nH2O [M = Ni, Cu; n = 0, 1], ML2·nH2O and ML′·nH2O [M = Co, Ni, Zn; HL′ = C6H5CH=CH-CH=N-NHC(O)NH2; n = 0–3]. In the presence of amines (A = C5H5N, 2-CH3C5H4N, 3-CH3C5H4N, and 4-CH3C5H4N) these reactions yield the complexes Cu(A)LCl·CH3OH and M(A)LX·nH2O [M = Cu, Ni; X = Cl, NO3; n = 0–2]. The copper complexes with the amine ligands are of polynuclear structure, and other complexes are monomeric. Carbazones (HL and HL′) are included in the complexes as bidentate N,S-and N,O-ligands. The thermolysis of the complexes involves the stages of removing solvent crystallization molecules (70–90°C), deaquation (150–170°C), and full thermal decomposition (500–580°C). 相似文献
10.
P. A. Abramov S. A. Adonin E. V. Peresypkina M. N. Sokolov V. P. Fedin 《Journal of Structural Chemistry》2010,51(4):731-736
Adducts of cucurbit[6]uril with Ca2+ and trinuclear cluster chloroaquacomplexes (H9O4)2(H7O3)2[(Ca(H2O)5)2(C36H36N24O12)]Cl8·0.67H2O (1) and [(Ca(H2O)5)2(C36H36N24O12)]× [Mo3O2S2Cl6(H2O)3]2·13H2O (2) are obtained and structurally characterized. The structures of both compounds contain polymeric [Ca(H2O)
n
]22 CB[6]∞ cations that form infinite columns; the space between them is filled with Cls- (1) and [Mo3O2S2Cl6(H2O)3]2s- (2). A new (H7O3)2(H5O2)× [Mo3S4Cl6.25Br0.25(H2O)2](C36H36N24O12)·CH2Cl2·6H2O complex (3) is also obtained and structurally characterized. 相似文献
11.
《Journal of Coordination Chemistry》2012,65(13):2095-2107
Several new coordination polymers of lanthanide tartrate with three types of topological structures, namely [Ln2(DL-tart)3(H2O)3] · 1.5H2O [Ln = La (1), Nd (2), and Sm (3)], [Ln2(D-tart)3(H2O)2] · 3H2O [Ln = Eu (4), Tb (5), and Dy (6)], and [Lu(C4H4O6)(C4H5O6)] · 2.5H2O (7), have been synthesized by hydrothermal synthesis. X-ray crystallographic analysis reveals that 1 is a unique 3-D network, whereas 5 with a 3-D network and 7 with a 2-D network are isomorphous with their analogs. All lanthanide ions are nine-coordinate through oxygen donors. Four different coordination modes of tartrate occur in these complexes. Luminescence spectra reveal that 4, 5, and 6 emit characteristic luminescence of corresponding lanthanide ions. 相似文献
12.
Rafael Cuesta Paloma Arranz‐Mascars John N. Low Christopher Glidewell 《Acta Crystallographica. Section C, Structural Chemistry》2001,57(8):918-921
In the title compound, [Na(C5H5N4O3)]·2H2O, each Na cation is linked to three C5H4N4O3? anions and two water molecules, forming approximately octahedral NaNO5 units; the cations and the anions form molecular ladders, and each ladder is linked to four neighbouring ladders by O—H?O and O—H?N hydrogen bonds. 相似文献
13.
Macromolecular Self‐Assembly of Organotin(IV) Squarates and Croconates – Preparation and Crystal Structures of [SnMe2(H2O)2]C4O4, [SnMe3]2C4O4, and [SnMe3(H2O)]2C5O5 下载免费PDF全文
Phil Liebing Asrial A. Husien Axel Fischer Eckhart Nietzschmann Frank T. Edelmann 《无机化学与普通化学杂志》2017,643(8):536-543
The new organotin(IV) squarates and croconates [SnMe2(H2O)2]C4O4 ( 1 ), [SnMe3]2C4O4 ( 2 ), and [SnMe3(H2O)]2C5O5 ( 3 ), were prepared by salt metathesis from the appropriate sodium salts, and characterized by single‐crystal X‐ray diffraction and infrared spectroscopy. While 1 and 2 are coordination polymers with bridging C4O42– anions, compound 3 exists as a monomer in the solid state. In the hydrated compounds 1 and 3 , the molecules are interconnected by various types of O–H ··· O bridges between non‐coordinated carbonyl oxygen atoms and water ligands, resulting in a supramolecular layer ( 1 , 2 ) or network structure ( 3 ), respectively. 相似文献
14.
Under hydrothermal conditions, four lanthanide coordination polymers were synthesized based on 4-(4,5-dicarboxy-1H-imidazol-2-yl)pyridine 1-oxide (H3DCImPyO), with the molecular forumulas [Eu(HDCImPyO)·(H2O)2·(CHO2)]n (1), [Sm(HDCImPyO)·(H2O)2·(HCO2)]n (2), {[La(HDCImPyO)·(H2O)·(HCO2)]·O2}n (3) and {[Y(HDCImPyO)·(C2O4)·(H2O)2]·H2O}n (4). With diverse coordination modes, they were further characterized by elemental analysis, infrared spectroscopy, dielectric measurement, and single-crystal X-ray structural analysis. Complexes 1 and 2 were isostructural and had similar structures with {44, 62} topology. Complex 1 exhibited strong fluorescent emission in the solid state at room temperature. In 3, HDCImPyO2? adopted μ4-kO, O′: kO′, O′′: O′′′: O′′′′ coordination to bridge four La(III) ions to form a 3-D framework with {4. 52}2{42. 510. 612. 7. 83} topology. In 4, both HDCImPyO2? ligands and Y3+ cations were simplified as linkers to form an interpenetrating 3-D framework with {413. 62}2{422. 66} topology. 相似文献
15.
Choudhury M. Zakaria George Ferguson Alan J. Lough Christopher Glidewell 《Acta Crystallographica. Section C, Structural Chemistry》2001,57(6):687-689
In the title compound, 2[Fe(C5H5)(C6H5O2)]·C6H12N2, the molecular components are linked into finite three‐component aggregates by strong O—H?N hydrogen bonds [O?N 2.578 (4) and 2.604 (5) Å; O—H?N 170 (5) and 174 (6)°]; these aggregates are further linked by C—H?O hydrogen bonds [C?O 3.327 (5)–3.401 (5) Å; C—H?O 149–157°] into continuous sheets in the form of (6,3) nets. 相似文献
16.
Selçuk Demir Günay Kaya Kantar Yıldıray Topcu Qiaowei Li 《Transition Metal Chemistry》2012,37(3):257-263
The complexes [Co(C4H4O4)]n (1) and [Zn(im)2(C4H4O4)]n
(2) (C4H4O4 = succinate dianion, suc; im = imidazole) have been synthesized solvothermally and characterized by elemental analysis, IR,
TG–DTA, and single-crystal X-ray diffraction techniques. Complex 1 is the first anhydrous member of the cobalt succinate family and has high thermal stability under a static air atmosphere,
up to 425 °C, and complex 2 is a 1D coordination polymer. In addition, a new synthesis method and some properties of the known [Co(HCOO)2·2H2O]n (3) complex are reported. After in situ synthesis of 3 via decomposition of DMF at 140 °C, it was found that complex 3 can adsorb some solvents repeatedly and is selective for H2O. 相似文献
17.
Reactions of a freshly prepared Zn(OH)2‐2x(CO3)x · yH2O precipitate, phenanthroline with azelaic and sebacic acid in CH3OH/H2O afforded [Zn(phen)(C9H15O4)2] ( 1 ) and [Zn2(phen)2(H2O)2(C10H16O4)2] · 3H2O ( 2 ), respectively. They were structurally characterized by X‐ray diffraction methods. Compound 1 consists of complex molecules [Zn(phen)(C9H15O4)2] in which the Zn atoms are tetrahedrally coordinated by two N atoms of one phen ligand and two O atoms of different monodentate hydrogen azelaato groups. Intermolecular C(alkyl)‐H···π interactions and the intermolecular C(aryl)‐H···O and O‐H···O hydrogen bonds are responsible for the supramolecular assembly of the [Zn(phen)(C9H15O4)2] complexes. Compound 2 is built up from crystal H2O molecules and the centrosymmetric binuclear [Zn2(phen)2(H2O)2(C10H16O4)2] complex, in which two [Zn(phen)(H2O)]2+ moieties are bridged by two sebacato ligands. Through the intermolecular C(alkyl)‐H···O hydrogen bonds and π‐π stacking interactions, the binuclear complex molecules are assembled into layers, between which the lattice H2O molecules are sandwiched. Crystal data: ( 1 ) C2/c (no. 15), a = 13.887(2), b = 9.790(2), c = 22.887(3)Å, β = 107.05(1)°, U = 2974.8(8)Å3, Z = 4; ( 2 ) P1¯ (no. 2), a = 8.414(1), b = 10.679(1), c = 14.076(2)Å, α = 106.52(1)°, β = 91.56(1)°, γ = 99.09(1)°, U = 1193.9(2)Å3, Z = 1. 相似文献
18.
《中国化学会会志》2017,64(1):43-54
White microcrystalline diamagnetic oxoperoxotungstate(VI) complexes K[WO(O2)2F]·H2O, K2[WO(O2)2(CO3)]·H2O, [WO(O2)(SO4)(H2O)2] have been synthesized from reaction of Na2WO4·2H2O with aqueous HF, solid KHCO3, aqueous H2SO4 (W:F− 1:3; W: CO3 2 − 1:1; and W: SO4 2 − 1:3), and an excess of 30% H2O2 at pH 7.5–8. Precipitation was completed by the addition of precooled acetone. The occurrence of terminal WO and triangular bidentate O2 2 −(C 2 v ) in the synthesized compounds was ascertained from IR spectra. The IR spectra also suggested that the F− and SO4 2 − ions in K[WO(O2)2F]·H2O and [WO(O2)(SO4)(H2O)2] were bonded to the WO +4 center in monodentate manner, while CO3 2 − ion in K2[WO(O2)2(CO3)]·H2O binds the metal center in bidentate chelating fashion. The complex [WO(O2)(SO4)(H2O)2] is stable upto 110°C. The water molecule in [WO(O2)(SO4)(H2O)2] is coordinated to the WO +4 center, whereas it occurs as water of crystallization in the corresponding peroxo(fluoro) and peroxo(carbonato) compounds. Mass spectra of the compounds are in good agreement with the molecular formulae of the complexes. K2[WO(O2)2(CO3)]·H2O acts as an oxidant for bromide in the aqueous‐phase bromination of organic substrates to the corresponding bromo‐organics, and the complex also oxidizes Hantzsch‐1,4‐dihydropyridine to the corresponding pyridine derivative in excellent yield at room temperature. Density functional theory computation was carried out to compute the frequencies of relevant vibrational modes and electronic properties, and the results are in agreement with the experimentally obtained data. 相似文献
19.
《Journal of Coordination Chemistry》2012,65(11):1233-1240
Reaction of freshly-prepared CuCO3, phenanthroline monohydrate and maleic acid in CH3OH/H2O(1 : 1 v/v) at pH=2.13 yielded diaqua(1,10-phenanthroline-N,N')hydrogenmaleatocopper(II) hydrogenmaleate monohydrate, [Cu(phen)(H2O)2(C4H3O4)](C4H3O4)(H2O), which consists of [Cu(phen)(H2O)2(C4H3O4)]+ complex cations, hydrogenmaleate anions and lattice H2O molecules. Within the complex cations, the Cu atoms are each square-pyramidally coordinated by two N atoms of one chelating phen ligand and three O atoms of two H2O molecules and one hydrogenmaleato ligand with one H2O molecule at the apical position (d(Cu-N) = 2.001, 2.009 Å, equatorial d(Cu-O) = 1.966 Å and axial d(Cu-O) = 2.235 Å). Through hydrogen bonding, the complex cations, hydrogenmaleate anions and lattice H2O molecules are assembled into 1D chains, which are held together by weak Cu···O interactions (3.139 Å) to form corrugated 2D layers. Significant π-π stacking interactions between neighboring phen ligands leads to supramolecular assembly of the 2D layers. Over the temperature range 5-300 K, the complex obeys the Currie-Weiss law with an effective magnetic moment of 1.78 BM at room temperature. 相似文献
20.
A. K. Molodkin N. Ya. Esina M. N. Kurasova 《Russian Journal of Inorganic Chemistry》2010,55(3):370-376
The complexation in iridium(IV)-purine base (adenine, hypoxanthine)-amino acid (α-alanine, aspartic acid, lysine) systems
was studied by pH titration. The stability constants of 1: 1: 1 complexes were determined. The stability of 1: 1: 1 mixed-ligand
complexes with hypoxanthine and adenine increases in the series Ala < Lys < Asp. Reactions between aqueous solutions gave
the following coordination compounds: [Ir(C5H4N4O)(C3H6NO2)Cl]Cl2, [Ir(C5H4N4O)(C4H5NO4)]Cl2, [Ir(C5H4N4O)(C6H13N2O2)]Cl3, [Ir(C5H5N5)(C3H6NO2)]Cl3, [Ir(C5H5N5)(C4H5NO4)]Cl2, and [Ir(C5H5N5)(C6H13N2O2)]Cl3. The individual character of the complexes was established by chemical and thermogravimetric analyses and powder X-ray diffraction.
The complexes were characterized by NMR, IR, and X-ray photoelectron spectroscopy. Alanine and lysine in mixed-ligand iridium(IV)
complexes are bidentate (α-NH2 and COO− groups), aspartic acid is tridentate, and purine bases function as polydentate ligands through heterocycle N atoms and functional
groups (NH2 in adenine and C=O in hypoxanthine). 相似文献