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1.
On the Crystal Structure of Melem C6N7(NH2)3 Single crystals of melem ( 1 ) were grown from both DMSO‐solutions and the gas phase. The structure of melem ( 1 ) was solved by single‐crystal X‐ray diffraction (P21/c, Z = 4, a = 741.66(15), b = 862.28(17), c = 1335.9(3) pm, β = 99.91(3)° R1 = 0.037 for 1098 reflections). The structure determination by X‐ray powder diffraction, which has been previously conducted, is in agreement with our data. The increased quality of the structural information allows for a more detailed understanding of the hydrogen bonding network. 相似文献
2.
Crystal Structure of Sodium Dihydrogencyamelurate Tetrahydrate Na[H2(C6N7)O3] · 4 H2O Sodium dihydrogencyamelurate‐tetrahydrate Na[H2(C6N7)O3]·4 H2O was obtained by neutralisation of an aqueous solution, previously prepared by hydrolysis of the polymer melon with sodium hydroxide. The crystal structure was solved by single‐crystal X‐ray diffraction ( a = 6.6345(13), b = 8.7107(17), c = 11.632(2) Å, α = 68.96(3), β = 87.57(3), γ = 68.24(3)°, V = 579.5(2) Å3, Z = 2, R1 = 0.0535, 2095 observed reflections, 230 parameters). Both hydrogen atoms of the dihydrogencyamelurate anion are directly bound to nitrogen atoms of the cyameluric nucleus, thus proving the preference of the keto‐tautomere in salts of cyameluric acid in the solid‐state. The compound forms a layer‐like structure with an extensive hydrogen bonding network. 相似文献
3.
We synthesized melemium hydrogensulfate H3C6N7(NH2)3(HSO4)3 by reaction of melem with 70 % sulfuric acid. The crystal structure was elucidated by single‐crystal XRD (P21/n (no. 14), Z = 4, a = 10.277(2), b = 14.921(3), c = 11.771(2) Å, β = 99.24(3)°, V = 1781.5(6) Å3). H3C6N7(NH2)3(HSO4)3 is the first compound displaying a triple protonation of melem., In this contribution an overview of accessible melemium sulfates depending on the concentration of sulfuric acid is given. Two additional melemium sulfates were identified this way. 相似文献
4.
Sophia J. Makowski Daniel Gunzelmann Jürgen Senker Wolfgang Schnick Prof. Dr 《无机化学与普通化学杂志》2009,635(15):2434-2439
Calcium hydrogenmelonate heptahydrate Ca[HC6N7(NCN)3] · 7H2O was obtained by metathesis reaction in aqueous solution. The structure of the molecular salt was elucidated by single‐crystal X‐ray diffraction. The crystal structure consists of alternating layers of planar monopronated melonate ions, Ca2+ and crystal water molecules. The anions of adjacent layers are staggered so that no π–π stacking occurs. The melonate entities are interconnected by hydrogen bonds within and between the layers. Ca[HC6N7(NCN)3] · 7H2O was investigated by solid‐state NMR and FTIR spectroscopy, TG and DTA measurements. 相似文献
5.
Interaction of copper(II) chloride with 2, 4, 6‐triallyloxy‐1, 3, 5‐triazine leads to formation of copper(II) complex [CuCl2·2C3N3(OC3H5)3] ( I ). Electrochemical reduction of I produces the mixed‐valence CuI, II π, σ‐complex of [Cu7Cl8·2C3N3(OC3H5)3] ( II ). Final reduction produces [Cu8Cl8·2C3N3(OC3H5)3]·2C2H5OH copper(I) π‐complex ( III ). Low‐temperature X‐ray structure investigation of all three compounds has been performed: I : space group P1¯, a = 8.9565(6), b = 9.0114(6), c = 9.7291(7) Å, α = 64.873(7), β = 80.661(6), γ = 89.131(6)°, V = 700.2(2) Å3, Z = 1, R = 0.0302 for 2893 reflections. II : space group P1¯, a = 11.698(2), b = 11.162(1), c = 8.106(1) Å, α = 93.635(9), β = 84.24(1), γ = 89.395(8)°, V = 962.0(5) Å3, Z = 1, R = 0.0465 for 6111 reflections. III : space group P1¯, a = 8.7853(9), b = 10.3602(9), c = 12.851(1) Å, α = 99.351(8), β = 105.516(9), γ = 89.395(8), V = 1111.4(4) Å3, Z = 1, R = 0.0454 for 4470 reflections. Structure of I contains isolated [CuCl2·2C3N3(OC3H5)3] units. The isolated fragment of I fulfils in the structure of II bridging function connecting two hexagonal prismatic‐like cores Cu6Cl6, whereas isolated Cu6Cl6(CuCl)2 prismatic derivative appears in III . Coordination behaviour of the 2, 4, 6‐triallyloxy‐1, 3, 5‐triazine moiety is different in all the compounds. In I ligand moiety binds to the only copper(II) atom through the nitrogen atom of the triazine ring. In II ligand is coordinated to the CuII‐atom through the N atom and to two CuI ones through the two allylic groups. In III all allylic groups and nitrogen atom are coordinated by four metal centers. The presence of three allyl arms promotes an acting in II and III structures the bridging function of the ligand moiety. On the other hand, space separation of allyl groups enables a formation of large complicated inorganic clusters. 相似文献
6.
Single crystals of Li4(PO2NH)4 · 4 H2O were obtained by dissolving LiOH and H4(PO2NH)4 · 2 H2O in water and subsequent precipitation with acetone and ethanol followed by slow evaporation of the solvents. The structure of Li4(PO2NH)4 · 4 H2O was solved by single‐crystal X‐ray methods ( (No. 2), a = 489.2(2), b = 853.2(2), c = 880.5(2) pm, α = 101.71(3), β = 102.39(3), γ = 94.88(3)°, Z = 1). The structure is composed of LiO4 tetrahedra and (PO2NH)44? ions. The P4N4 rings of the anions exhibit a slightly distorted chair–1 conformation, which is supported by IR data and has been described by torsion angles, displacement asymmetry parameters and puckering parameters. Via Li+ ions and hydrogen bonds, the tetrametaphosphimate anions are connected forming a three‐dimensional network. 相似文献
7.
Synthesis and Crystal Structure of Ammonium Tetraamminelithium Amidotrithiophosphate‐Ammonia(1/1)(NH4)[Li(NH3)4][P(NH2)S3]·NH3 Colourless crystals of (NH4)[Li(NH3)4][P(NH2)S3]·NH3 were prepared by the reduction of P4S10 with a solution of lithium in liquid ammonia. The X‐ray structure determination shows them to contain the pseudo‐tetrahedral amidotrithiophosphate anion [P(NH2)S3]2− (point group CS), which is the hitherto unknown final member of a series of previously characterized amidothiophosphates. The ammonium ion and the ammonia molecule of solvation form an diamminehydrogen(1+)‐ion N2H7+ with a short, nearly linear hydrogen bond of 2.864(3) Å. 相似文献
8.
Phase‐pure ammonium catena‐polyphosphate IV [NH4PO3]x was synthesized by heating NH4H2PO4 in a tube furnace under an ammonia gas flow. The product contained single crystals of [NH4PO3]x IV appropriate for an X‐ray structure determination enabling structure refinement of this compound. The pseudo‐merohedrally twinned crystals of [NH4PO3]x crystallize in the monoclinic crystal system (P21/c, no. 14, a = 2270.3(5), b = 458.14(9), c = 1445.1(3) pm, β = 108.56(3)°, Z = 4, 2264 data, R1 = 0.076). In the unit cell the catena‐polyphosphate chain anions run parallel [010] with a chain‐periodicity P = 2 and a stretching factor fs = 0.94. The chain anions are interconnected through extensive hydrogen bonding towards the ammonium ions. Due to ‘chemical twinning’ a novel catena‐polyphosphate structure type is realized in [NH4PO3]x IV. The vibrational spectra of [NH4PO3]x IV are reported as well. 相似文献
9.
Several rare‐earth cyclotriphosphate hydrates were obtained from mixtures of sodium cyclotriphosphates and the respective rare‐earth chlorides. Nd(P3O9) · 3H2O [P$\bar{6}$ , Z = 3, a = 677.90(9), c = 608.67(9) pm, R1 = 0.016, wR2 = 0.038, 312 data, 36 parameters] was obtained by a solid state reaction and is isotypic with respective rare‐earth phosphate hydrates, while all the others adopt new structure types. Nd(P3O9) · 4.5H2O [C2/c, Z = 8, a = 1644.6(3), b = 756.11(15), c = 1856.1(4) pm, β = 97.25(3)°, R1 = 0.032, wR2 = 0.081, 1763 data, 194 parameters], Nd(P3O9) · 5H2O [P21/c, Z = 4, a = 773.75(15), b = 1149.1(2), c = 1394.9(3) pm, β = 106.07(3)°, R1 = 0.042, wR2 = 0.082, 1338 data, 194 parameters], Pr(P3O9) · 5H2O [P$\bar{1}$ , Z = 2, a = 745.64(15), b = 889.07(18), c = 934.55(19) pm, α = 79.00(3), β = 80.25(3), γ = 66.48(3), R1 = 0.059, wR2 = 0.089, 1468 data, 193 parameters], Na3Nd(P3O9)2 · 6H2O [P21/n, Z = 4, a = 1059.78(18), b = 1207.25(15), c = 1645.7(4) pm, β = 99.742(17), R1 = 0.047, wR2 = 0.119, 1109 data, 351 parameters] and Na3Pr(P3O9)2 · 6H2O [P21/n, Z = 4, a = 1061.42(16), b = 1209.0(2), c = 1635.5(3) pm, β = 99.841(13), R1 = 0.035, wR2 = 0.062, 1323 data, 350 parameters] were obtained by careful crystallization at room temperature. A thorough structure discussion is given. The infrared spectrum of Nd(P3O9) · 4.5H2O is also reported. 相似文献
10.
Preparation and Crystal Structures of the first Alkalimetall‐hexacarbonato‐oxotetraberyllates: K6[Be4O(CO3)6] · 7 H2O and K6[Be4O(CO3)6] K6[Be4O(CO3)6] · 7 H2O has been prepared by dissolving freshly precipitated Be(OH)2 in an aqueous KHCO3 solution. After enriching the title compound by extraction with ethanol the heptahydrate crystallizes from the organic phase (triklin, P1¯ (No. 2) with a = 951, 01(11), b = 958, 45(12), c = 1601, 7(2) pm, α = 79, 253(13)°, β = 78, 943(12)°, γ = 65, 119(12)°, VEZ = 1290, 6(3)·106 pm3, Z = 2). Thermal decomposition forms rhombohedral crystals of the anhydrous compound (trigonal‐rhombohedric, R3¯ (No. 148) with a = 1416, 42(6), c = 1704, 5(1) pm, VEZ = 2961, 4(3)·106 pm3, Z = 6). 相似文献
11.
Preparation, Crystal Structure, Thermal Decomposition, and Vibrational Spectra of [Co(NH3)6]2[Be4O(CO3)6] · 10 H2O [Co(NH3)6]2[Be4O(CO3)6] · 10 H2O is a suitable compound for the quantitative determination of beryllium. It can be obtained by reaction of aqueous solutions of carbonatoberyllate with [Co(NH3)6]Cl3. The crystal structure (trigonal‐rhombohedral, R3c (Nr. 161), a = 1071,6(1) pm, c = 5549,4(9) pm, VEZ = 5519(1) · 106 pm3, Z = 6, R1(I ≥ 2σ(I)) = 0,037, wR2(I ≥ 2σ(I)) = 0,094) contains [Co(NH3)6]3+‐ and [Be4O(CO3)6]6–‐ions, which are directly hydrogen bonded as well as with water molecules. The complex cations and anions occupy the positions of a distorted anti‐CaF2‐type. The thermal decomposition, IR and Raman spectra are presented and discussed. 相似文献
12.
Crystal Structure, Vibrational Spectra, and Normal Coordinate Analysis of ( n ‐Bu4N)2[{Ru(NO)ClI2}2(μ‐I2)] · 2 I2 By treatment of (n‐Bu4N)2[Ru(NO)I5] with (n‐Bu4N)Cl in dichloromethane (n‐Bu4N)2[{Ru(NO)ClI2}2(μ‐I2)] is formed. The X‐Ray structure determination on a single crystal of (n‐Bu4N)2[{Ru(NO)ClI2}2(μ‐I2)] · 2 I2 (monoclinic, space group I 2/a, a = 20.446(6), b = 11.482(8), c = 27.225(3) Å, β = 107.51(4)°, Z = 4) reveals a dinuclear iodine bridged structure, in which the chlorine atoms are trans positioned to the nitrosyl groups. The low temperature IR and Raman spectra have been recorded of (n‐Bu4N)2[{Ru(NO)ClI2}2(μ‐I2)] · 2 I2 and are assigned by normal coordinate analysis. A good agreement between observed and calculated frequencies is achieved. The valence force constants are fd(NO) = 14.08, fd(RuN) = 5.58, fd(RuCl) = 1.52, fd(RuIt) = 0.90 and fd(RuIb) = 0.76 mdyn/Å. 相似文献
13.
14.
(PPh4)2HP7 · 3NH3 was prepared by the reaction of K3P7 with a proton‐charged ion exchange resin in the presence of (PPh4)Br in liquid ammonia, and characterized by low temperature X‐ray structure analysis. The thermally very unstable compound contains the hydrogenheptaphosphide anion HPequation/tex2gif-stack-1.gif, the nortricyclane‐like cage of which is slightly distorted by the attachment of the hydrogen atom. 相似文献
15.
Andreas Fischer 《无机化学与普通化学杂志》2003,629(6):1012-1016
By slow evaporation of solutions containing UO2(ClO4)2 and an excess of HClO4, single crystals of [UO2(ClO4)2(H2O)3] ( 1 ) and [UO2(H2O)5](ClO4)2 ( 2 ) were obtained and their structures were determined. From similar solutions prepared from stoichiometric amounts of UO3 and perchloric acid, crystals of [UO2(H2O)5](ClO4)2·2H2O ( 3 ) were obtained. The trihydrate (monoclinic, P21/c, a = 545.44(1) pm, b = 1811.09(5) pm, c = 1032.46(2) pm, β = 90.016(1)°) consists of uranyl ions, which are coordinated by two monodentate perchlorate ions and three water molecules. The pentahydrate (monoclinic, P21/n, a = 529.35(2) pm, b = 1645.43(6) pm, c = 1480.18(6) pm, β = 99.847(1)°) contains uranyl ions coordinated by five water molecules. The same structural unit can be found in the heptahydrate, whose structure was re‐determined (orthorhombic, Pbcn, a = 920.9(3) pm, b = 1067.9(3) pm, c = 1445.7(3) pm). In this structure, two molecules of water of crystallization are present. 相似文献
16.
Diammonium tricyanomelaminate dihydrate [NH4]2[C6N9H] · 2 H2O ( 1 ) and dimelaminium tricyanomelaminate melamine dihydrate [C3N6H7]2[C6N9H] · C3N6H6 · 2 H2O ( 2 ) were obtained by metathesis reactions from Na3[C6N9] in aqueous solution and characterized by single‐crystal X‐ray diffraction and 15N solid‐state NMR spectroscopy ( 1 ). Both salts contain mono‐protonated tricyanomelaminate (TCM) anions and crystallize as dihydrates. Considering charge balance requirements, the crystal structure of 1 (C2/c, a = 3181.8(6) pm, b = 360.01(7) pm, c = 2190.4(4) pm, β = 112.39(3)°, V = 2319.9(8) 106 · pm3) can best be described by assuming a random distribution of an ammonium ion – crystal water pair over two energetically similar sites. Apart from two melaminium cations, 2 (P21/c, a = 674.7(5) pm, b = 1123.6(5) pm, c = 3400.2(5) pm, β = 95.398(5), V = 2566(2) 106 · pm3) contains one neutral melamine per formula unit acting as an additional “solvent” molecule and yielding a donor‐acceptor type of π–stacking interaction. 相似文献
17.
Synthesis, Crystal Structure, and Vibrational Spectra of cis ‐(CH2Py2)[ReBr4Py2]2 · (CH3)2CO By reaction of (n‐Bu4N)2[ReBr6] with pyridine and (n‐Bu4N)BH4 in dichloromethane halogeno‐pyridine‐rhenium(III)complexes are formed and purified by chromatography. X‐ray structure determination on a single crystal has been performed of cis‐(CH2Py2)[ReBr4Py2]2 · (CH3)2CO (monoclinic, space group P21/c, a = 15.0690(9), b = 8.3337(8), c = 35.588(4) Å, β = 96.409(7), Z = 4). Based on the molecular parameters of the X‐ray structure determination and assuming C2 point symmetry for the anion cis‐[ReBr4Py2]– the IR and Raman spectra are assigned by normal coordinate analysis. The valence force constants are in the Br–Re–Br axis fd(ReBr) = 1.49, in the asymmetrically coordinated N′–Re–Br · axes fd(ReBr · ) = 1.03 und fd(ReN′) = 2.52 mdyn/Å. 相似文献
18.
The compound [NH4(NH3)4][Co(C2B9H11)2] · 2 NH3 ( 1 ) was prepared by the reaction of Na[Co(C2B9H11)2] with a proton‐charged ion‐exchange resin in liquid ammonia. The ammoniate 1 was characterized by low temperature single‐crystal X‐ray structure analysis. The anionic part of the structure consists of [Co(C2B9H11)2]‐ complexes, which are connected via C‐H···H‐B dihydrogen bonds. Furthermore, 1 contains an infinite equation/tex2gif-stack-2.gif[{NH4(NH3)4}+(μ‐NH3)2] cationic chain, which is formed by [NH4(NH3)4]+ ions linked by two ammonia molecules. The N‐H···N hydrogen bonds range from 1.92 to 2.71Å (DHA = Donor···Acceptor angles: 136‐176°). Additional N‐H···H‐B dihydrogen bonds are observed (H···H: 2.3‐2.4Å). 相似文献
19.
Torsten Küppers Martin Köckerling Prof. Dr. Helge Willner Prof. Dr. 《无机化学与普通化学杂志》2007,633(2):280-284
The new tetracyanoborate K[B(CN)4]·CH3CN was synthesized by dissolution of the solvent‐free K[B(CN)4] in acetonitrile and subsequent careful crystallization. The crystal structure has been determined by single‐crystal X‐ray diffraction. It crystallizes in the orthorhombic space group P212121 with Z = 4. Some comparisons with related structures are made, and the vibrational spectrum is discussed. 相似文献
20.
The new hexathiodiphosphate(IV) hydrates K4[P2S6] · 4 H2O ( 1 ), Rb4[P2S6] · 6 H2O ( 2 ), and Cs4[P2S6] · 6 H2O ( 3 ) were synthesized by soft chemistry reactions from aqueous solutions of Na4[P2S6] · 6 H2O and the corresponding heavy alkali‐metal hydroxides. Their crystal structures were determined by single crystal X‐ray diffraction. K4[P2S6] · 4 H2O ( 1 ) crystallizes in the monoclinic space group P 21/n with a = 803.7(1), b = 1129.2(1), c = 896.6(1) pm, β = 94.09(1)°, Z = 2. Rb4[P2S6] · 6 H2O ( 2 ) crystallizes in the monoclinic space group P 21/c with a = 909.4(2), b = 1276.6(2), c = 914.9(2) pm, β = 114.34(2)°, Z = 2. Cs4[P2S6] · 6 H2O ( 3 ) crystallizes in the triclinic space group with a = 742.9(2), b = 929.8(2), c = 936.8(2) pm, α = 95.65(2), β = 112.87(2), γ = 112.77(2)°, Z = 1. The structures are built up by discrete [P2S6]4? anions in staggered conformation, the corresponding alkali‐metal cations and water molecules. O ··· S and O ··· O hydrogen bonds between the [P2S6]4? anions and the water molecules consolidate the structures into a three‐dimensional network. The different water‐content compositions result by the corresponding alkali‐metal coordination polyhedra and by the prefered number of water molecules in their coordination sphere, respectively. The FT‐Raman and FT‐IR/FIR spectra of the title compounds have been recorded and interpreted, especially with respect to the [P2S6]4? group. The thermogravimetric analysis showed that K4[P2S6] · 4 H2O converted to K4[P2S6] as it was heated at 100 °C. 相似文献