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1.
The Reactions of M[BF4] (M = Li, K) and (C2H5)2O·BF3 with (CH3)3SiCN. Formation of M[BFx(CN)4—x] (M = Li, K; x = 1, 2) and (CH3)3SiNCBFx(CN)3—x, (x = 0, 1) The reaction of M[BF4] (M = Li, K) with (CH3)3SiCN leads selectively, depending on the reaction time and temperature, to the mixed cyanofluoroborates M[BFx(CN)4—x] (x = 1, 2; M = Li, K). By using (C2H5)2O·BF3 the synthesis yields the compounds (CH3)3SiNCBFx(CN)3—x x = 0, 1. The products are characterized by vibrational and NMR‐spectroscopy, as well as by X‐ray diffraction of single‐crystals: Li[BF2(CN)2]·2Me3SiCN Cmc21, a = 24.0851(5), b = 12.8829(3), c = 18.9139(5) Å V = 5868.7(2) Å3, Z = 12, R1 = 4.7%; K[BF2(CN)2] P41212, a = 13.1596(3), c = 38.4183(8) Å, V = 6653.1(3) Å3, Z = 48, R1 = 2.5%; K[BF(CN)3] P1¯, a = 6.519(1), b = 7.319(1), c = 7.633(2) Å, α = 68.02(3), β = 74.70(3), γ = 89.09(3)°, V = 324.3(1) Å3, Z = 2, R1 = 3.6%; Me3SiNCBF(CN)2 Pbca, a = 9.1838(6), b = 13.3094(8), c = 16.840(1) Å, V = 2058.4(2) Å3, Z = 8, R1 = 4.4% 相似文献
2.
The reactions of CF3I(Cl)F and CF3IF2 with (CH3)3SiOCH3 lead to the novel iodine(III) compounds CF3I(Cl)OCH3 and CF3I(OCH3)2, respectively. The crystal structure of CF3I(Cl)OCH3 confirms that it is a ternary, trifluoromethyl-substituted iodine(III) derivative. CF3I(Cl)OCH3 crystallizes in the triclinic space group P1¯, with four formula units per unit cell with the dimensions a = 8.164(1), b = 8.802(1), c = 10.237(1) Å and angles α = 97.10(1)°, β = 91.41(1)°, γ = 115.00(1)°. CF3I(OCH3)2 crystallizes in the monoclinic space group P21/n with four formula units per unit cell with a = 6.295(1), b = 15.607(1), c = 7.736(1) Å, and β= 111.44(1)°. Both molecules have been additionally characterized by Raman, IR, and NMR spectroscopy and the experimental results are compared with quantum-mechanically calculated parameters. 相似文献
3.
Michael Berkei Eduard Bernhardt Markus Schürmann Michael Mehring Helge Willner 《无机化学与普通化学杂志》2002,628(8):1734-1740
Preparation, Spectroscopic Characterization and Crystal Structures of Mercury(II)‐bis(tetracyanoborate) Hg[B(CN)4]2 and Dimercury(I)‐bis(tetracyanoborate) Hg2[B(CN)4]2 Hg[B(CN)4]2 ( 1 ) is synthesised by the reaction between Hg(NO3)2 and K[B(CN)4]2. In a comproportionation reaction of 1 with elemental mercury the corresponding mercury(I) salt Hg2[B(CN)4]2 ( 2 ) is obtained. The compounds were characterised by vibrational‐ and NMR‐spectroscopy, and their crystal structures were determined. Hg[B(CN)4]2 crystallizes in the trigonal system in the space group P3¯m1 with a = 781.75(3) pm, c = 601.68(2) pm, V = 318.44(2)Å3, and one formula unit per unit cell. For Hg2[B(CN)4]2 an orthorhombic unit cell with a = 568.9(1) pm, b = 3280.9(7) pm, c = 601.68(2) pm, V = 1389.6(5)Å, and Z = 4 is observed. 相似文献
4.
Spectroscopic Characterization and Crystal Structure of Trifluoromethyl Iodine(III) Chloride Trifluororacetate (CF3I(Cl)OCOCF3) The ternary iodine(III) compound CF3I(Cl)OCOCF3 is obtained by reaction between CF3I(Cl)F and (CH3)3SiOCOCF3 at –50 °C. The molecule was characterized by vibrational spectra, NMR‐spectra, and a crystal structure analysis. CF3I(Cl)OCOCF3 crystallizes monoclinic in the space group P21/c with a = 1102.7(1) pm, b = 785.6(1) pm, c = 989.7(1) pm, and β = 101.34(1)°. 相似文献
5.
Karolina Kazmierczak 《Journal of solid state chemistry》2010,183(9):2087-2094
The potassium lanthanide double sulphates KLn(SO4)2·H2O (Ln=La, Nd, Sm, Eu, Gd, Dy) were obtained by evaporation of aqueous reaction mixtures of rare earth (III) sulphates and potassium thiocyanate at 298 K. X-ray single-crystal investigations show that KLn(SO4)2·H2O (Ln=Nd, Sm, Eu, Gd, Dy) crystallise monoclinically (Ln=Sm: P21/c, Z=4, a=10.047(1), b=8.4555(1), c=10.349(1) Å, wR2=0.060, R1=0.024, 945 reflections, 125 parameters) while KLa(SO4)2·H2O adopts space group P3221 (Z=3, a=7.1490(5), c=13.2439(12) Å, wR2=0.038, R1=0.017, 695 reflections, 65 parameters). The coordination environment of the lanthanide ions in KLn(SO4)2·H2O is different in the case of the Nd/Sm/Gd and the Eu/Dy compounds, respectively. In the first case the Ln atoms are nine-fold coordinated in contrast to the latter where the Ln ions are eight-fold coordinated by oxygen atoms. The vibrational spectra of KLn(SO4)2·H2O and the UV-vis reflection spectra of KEu(SO4)2·H2O and KNd(SO4)2·H2O are also reported. 相似文献
6.
Srinivasan Natarajan Yurii Prots Bastian Ewald Rainer Niewa Rüdiger Kniep 《无机化学与普通化学杂志》2006,632(1):37-41
Two polymorphs of a zero‐dimensional (molecular) zinc phosphate with the formula [Zn(2,2′‐bipy)(H2PO4)2]2 have been synthesized by a mild hydrothermal route and their crystal structures were determined by single crystal X‐ray diffraction (triclinic, space group (No. 2), Z = 2, α‐form: a = 8.664(1), b = 8.849(2), c = 10.113(2) Å, α = 97.37(2)°, β = 100.54(2)°, γ = 100.98(2)°, V = 737.5(3) Å3; β‐form: a = 7.5446(15), b = 10.450(2), c = 10.750(2) Å, α = 67.32(3)°, β = 81.67(3)°, γ = 69.29(3)°, V = 731.4(3) Å3). Both structures consist of distorted trigonal‐bipyramidal ZnO3N2 units condensed with PO2(OH)2 tetrahedra through common vertices giving rise to dimers [Zn(2,2′‐bipy)(H2PO4)2]2. The structures are stabilized by extensive inter‐ and intramolecular hydrogen bond interactions. Both modifications display subtle differences in their packing originating from the hydrogen bond interactions as well as π…π interactions between the organic ligands. 相似文献
7.
The crystal structure of the novel iodine compound Cl2IOI(O)F2 is described. Cl2IOI(O)F2 contains iodine in two different oxidation states (III) and (V) and can formally be described as ICl2+IF2O2−, linked by an unsymmetrical, nonlinear I−O−I bridge, with I−O bond lengths of 1.84(1) Å and 2.32(1) Å, and a bond angle of 122.5(5)°. It was accidentally obtained by the uncontrolled reaction between CF3I, CF3OCl, CF2O, and Cl2 at −70 °C over a period of about six months and finally two days at room temperature. Cl2IOI(O)F2 crystallises in the monoclinic space group P21/c with four formula units per unit cell with the dimensions a = 12.910(1), b = 6.987(1), c = 7.550(1) Å, and β = 94.890(1)°. The molecule was additionally characterised by its Raman and IR spectra. 相似文献
8.
Structure and Properties of the Methyltetrafluorophosphate Anion, [CH3PF5]— Methyltetrafluorphosphorane reacts with the fluorides NaF, KF, CsF, and (CH3)4NF with formation of the corresponding methylpentafluorophosphates. In case of the K and Cs salts K[CH3PF5] · CH3CN and Cs[CH3PF5] · CH3CN, respectively, are formed using acetonitrile as solvent. The salts are characterized by NMR, IR and Raman spectroscopy. The vibrational frequencies are compared with ab initio calculated data (RHF/6‐31+G*). The RHF/6‐31+G* calculation yields for the almost octahedral anion bond distances of d(PFeq) = 163.7 pm, d(PFax) = 162.0 pm, and d(PC) = 184.8 pm. 相似文献
9.
The crystal structure of [{Fe(CO)4}2(μ-η2:2-s-trans-C4H6)] was determined by single-crystal X-ray diffraction at 90 K. The complex is located on a center of symmetry in the triclinic space group P1‾. The central C-C bond of the s-trans-butadiene ligand is slightly longer compared to non-coordinated s-trans-butadiene. The Fe-Cax bond lengths are slightly longer than d(Fe-Ceq) in agreement with marginally shorter d(C≡Oax) compared to d(C≡Oeq). In addition, the title complex was characterized by IR and Raman as well as NMR spectroscopy and the data are interpreted by the aid of results of DFT calculations. 相似文献
10.
The vibrational properties of fluorocarbonyl peroxynitrate, FC(O)OONO2 and chlorocarbonyl peroxynitrate, ClC(O)OONO2 were studied by means of density functional theory (DFT) methods. The obtained results served to revise the reported experimental spectra and their corresponding assignments. Subsequently, the revised data were used in the definition of scaled quantum mechanics (SQM) force fields for these peroxynitrates. A set of internal force constants was also calculated from such force fields. 相似文献
11.
12.
The low-temperature form of K3Sm(PO4)2 crystallizes in the monoclinic system [a = 7.4347(5) Å, b = 5.6270(5) Å, c = 9.4919(5) Å, β = 90.870(6)°, Z = 2, space group P21/m]. The structure has been determined using 1263 independent reflections (R = 0.045, Rw = 0.11) and is found to be of the glaserite type. The Raman and infrared spectra have been investigated: they are consistent with the proposed space group and an assignment of the observed frequencies is given. 相似文献
13.
Fengjiao Guo;Jian Han;Jianian Cheng;Zhihua Yang;Tushagu Abudouwufu;Hongwei Yu;Shilie Pan; 《欧洲无机化学杂志》2019,2019(19):2462-2467
Two phosphates, Cs2Zn5(PO4)4 and Cs3La(PO4)2 have been successfully synthesized by employing the conventional solid-state reaction method, and their structures were determined by single-crystal X-ray diffraction. Cs2Zn5(PO4)4 owns a three-dimensional ∞3[Zn4P4O16] framework and Cs3La(PO4)2 features ∞2[La3P6O29] layers spreading in the bc plane. Infrared spectroscopy, UV/Vis-NIR diffuse reflectance spectroscopy were performed. The thermal properties and electronic structures of two compounds were investigated. In addition, the Ce3+ doped Cs3La(PO4)2 phosphor was synthesized and its photoluminescence was analyzed. The results indicate that the Cs2Zn5(PO4)4:0.01Ce3+ phosphor can be excited by ultraviolet light to obtain blue luminescence. 相似文献
14.
Ba(CF3SO3)2 reacts with the O‐donor ligand THF to yield the coordination compound {[Ba(OTf)2(thf)3]2[Ba(OTf)2(thf)2]} ( 1 ) (OTf = CF3SO3–). The title compound can be described as a one‐dimensional excerpt from the higher‐dimensional crystal structure of Ba(CF3SO3)2, stabilized by THF. This example for the concept of formally “cutting out” structural elements from a three‐dimensional solid state compound confirms and can be compared to the case of the structural “genealogy tree” of BaI2. This could be an efficient approach for new materials with highly anisotropic properties. 相似文献
15.
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
16.
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
17.
Single crystals of [Yb(NCS)3(H2O)5] · H2O were synthesized from a salt‐metathesis reaction between stoichiometric amounts of aqueous solutions of Yb2(SO4)3 · 8H2O and Ba(NCS)2 · 3H2O driven by the precipitation of Ba(SO4), followed by isothermic evaporation of the filtered‐off solution at room temperature under atmospheric conditions. These crystals of the title compound came as transparent, colorless and hygroscopic needles. According to the X‐ray diffraction structure analysis [Yb(NCS)3(H2O)5] · H2O crystallizes in the monoclinic space group P21 with the lattice parameters a = 845.38(5), b = 719.26(4), c = 1219.65(7) pm, β = 103.852(3)° for Z = 2. The acentric crystal structure contains crystallographically unique Yb3+ cations, each surrounded by three thiocyanate anions, all grafting with their nitrogen atoms, and five water molecules forming a neutral [Yb(NCS)3(H2O)5] complex with square antiprismatic shape, completed by a sixth interstitial water molecule. ATR‐FT infrared and single‐crystal Raman spectra of [Yb(NCS)3(H2O)5] · H2O confirm these findings. 相似文献
18.
Two new borosulfates were obtained either by an open vessel synthesis from sulfuric acid and B(OH)3, yielding (NH4)3[B(SO4)3] or from solvothermal synthesis in oleum enriched sulfuric acid and B(OH)3, yielding Sr[B2(SO4)4]. (NH4)3[B(SO4)3] crystallizes homeotypic to K3[B(SO4)3] in space group Ibca (Z = 8, a = 728.58(3) pm, b = 1470.84(7) pm, c = 2270.52(11) pm), comprising open branched vierer single chains {1∞[B(SO4)2(SO4)2/2]3–}. Sr[B2(SO4)4] crystallizes as an ordered variant of Pb[B2(SO4)4] in space group Pnna (Z = 4, a = 1257.4(4) pm, b = 1242.1(4) pm, c = 731.9(2) pm), consisting of loop branched vierer single chains {1∞[B(SO4)4/2]2–}. Vibrational spectroscopy confirms both refined structure models. Thermal analysis of the dried powders, showed a decomposition towards the binary and ternary components, whereas a thermal treatment in the presence of the mother liquor promotes a decomposition of Sr[B2(SO4)4] towards Sr[B2O(SO4)3]. 相似文献
19.
Marcel J. J. Blommers Wolfgang Jahnke 《Angewandte Chemie (International ed. in English)》1998,37(4):456-458
Help in determining biomolecular structure by NMR spectroscopy is found in a new method recently proposed by Reif, Hennig, and Griesinger, which enables the direct measurement of angles between bond vectors (see picture; X, Y=13C, 15N). This work may be another milestone in the progress of NMR spectroscopy toward simpler and more generally applicable structure determination of biomolecules. 相似文献
20.
Mark T. Weller Maria J. Pack Norman Binsted 《Angewandte Chemie (International ed. in English)》1998,37(8):1094-1097