Crystal Structure Of Cs Research Articles

Preparation and X-ray crystal structure of caesium imidodisulphuryl fluoride Cs[N(SO 2F) 2

The salt Cs[N(SO 2F) 2] was prepared from a stoichiometric reaction of imidodisulphuryl fluoride, HN(SO 2F) 2, and caesium hydroxide in high yield. The crystal structure of Cs[N(SO 2F) 2] was determined at room temperature. The compound is monoclinic, space group P2 1 n , with four molecules in a unit cell of dimensions a = 7.884 0(3) Å, b = 8.455 0(5) Å, c = 10.659 0(5) Å, and β = 99.621 (4)° with R = 0.024, R w 2 = 0.066, for 1234 observed [ I>2 δ( I)] reflections (for all data: R = 0.025, R w 2 = 0.074). The nitrogen atom in the anionic moiety [N(SO 2F) 2] − has trigonal planar coordination geometry with an S-N-S angle of 120.8(2)°.

Cs3Zr7Cl20Mn: A Zirconium Cluster Network Compound with Isolated ZrCl5- Units in a Stuffed Perovskite Structure

Reactions of Zr, ZrCl{sub 4}, and MnCl{sub 2} in welded Ta containers at 800 {degrees}C produce the title phase in major amounts. A comparable electronic and structural configuration is also found with interstitial boron, but not in isostructural compounds with other interstitial or alkali metal atoms. The crystal structure of Cs{sub 3}(ZrCl{sub 5})[Zr{sub 6}(Mn)Cl{sub 12}]Cl{sub 6/2} was established by single-crystal diffraction (R3c, Z = 6, a = 12.8924(1) {angstrom}, c = 35.187 (6) {angstrom}, R/R{sub w} = 1.9/2.3% for 920 data to 20 = 60{degrees}). The structure contains a three-dimensional array of 18-electron Zr{sub 6}(Mn)Cl{sub 12} clusters interbridged by 6/2 Cl{sup a-a} atoms at zirconium vertices. This represents a sixth independent structure type for M{sub 6}X{sub 15} bridged cluster networks. The structure derives from a ReO{sub 3}-like primitive lattice of the cubic Nb{sub 6}F{sub 15} structure with linear bridges that has been given a {open_quotes}trigonal twist{close_quotes} about [111] to form a rhombohedral (tilted) perovskite arrangement with the novel ZrCl{sub 5}{sup {minus}} at the body center. This new D{sub 3h} anion does not share halogen with the rest of the structure and appears to be stabilized by a particularly good fit within the network. A double ccp cluster arrangement along c{submore » H} provides for a coherent intercluster bridging arrangement. The cesium cations necessitated by the anionic network and by the CsZrCl{sub 5} component are bound in well-suited 12-coordinate sites among the chlorines.« less

Darstellung, 11B-NMR- und Schwingungsspektren von Aminohexahydro-closo-hexaborat(1–), [B6H6(NH2)]- sowie Kristallstruktur von Cs[B6H6(NH2)] · H2O / Preparation, 11B NMR and Vibrational Spectra of Aminohexahydro-closo-hexaborate(1–), [B6H6(NH2)]-, and the Crystal Structure of Cs[B6H6(NH2)] · H2O

Aminohexahydro-closo-hexaborate(1–), Crystal Structure, 11B NMR Spectra, Vibrational Spectra By reduction of [B6H5(NO2)]2- with Fe2+ in aqueous alkaline solution [B6H6(NH2)]- is formed. The compound has been separated by extraction with dichloromethane in the presence of tetrabutylammoniumbromid and precipitated from the organic phase by adding CsCH3COO/C2H5OH. The Crystal structure of Cs[B6H6(NH2)] · H2O has been determined by single crystal X-ray diffraction analysis; monoclinic space group C2 with a = 22.1075(14), b = 6.491(2), c = 5.9570(4) A, β = 100.168(6)°. The 11B NMR spectrum is consistent with a mono-hetero-substituted octahedral B6 cage with local C4v symmetry. The IR and Raman spectra exhibit characteristic N–H, B–H and B6 vibrations.

Darstellung, 11B-, 13C-NMR-und Schwingungsspektren von Aminom ethylhexahydro-closo-hexaborat(1-), [B6H6(CH2NH2)]- sowie Kristallstrukturen von Cs[B6H6(CH2NH2)] und K[B6H6(CH2NH2)] / Preparation, 11B, 13C NMR and Vibrational Spectra of Aminomethylhexahydro-closo-hexaborate(1-), [B6H6(CH2NH2)]-, and Crystal Structures of Cs[B6H6(CH2NH2)] and K[B6H6(CH2NH2)

By reaction of [B6H6]2- with N-(chloromethyl)phthalimide in dichloromethane the intermediate phthalimidomethylhexahydro-closo-hexaborate(1-), [B6H6(CH2(NC8O2H4)]-, is formed which with an excess of hydrazine reacts to give am inomethylhexahydro-closo-hexaborate(1-). The crystal structures of Cs[Bf,H6(CH2NH2)] and K[B6H6(CH2NH2)] have been determined by single crystal X -ray diffraction analysis. They are monoclinic, space group C2/m with a = 11.123(6), b = 6.8441(11), c = 12.810(7) Å, β = 124.032(5)° for Cs[B6H6(CH2NH2)] and with a = 10.767(2), b = 6.6255(6), c = 12.2648(14) Å, β = 123.880(10")° for K [B6H6(CH2NH2)]. The 11B NMR spectrum is consistent with a monohetero substituted octahedral B6 cage with local C4v symmetry. In the 13C NMR spectrum of Cs[B6H6(CH2NH2)] a quartet at 32.7 ppm with 1J(C,B) 65 Hz is observed. The IR and Ram an spectra exhibit characteristic CH, NH, BH and B6 vibrations

Darstellung, 11B-, 13C-NMR- und Schwingungsspektren der closo-Hexaborate [B6H5(CN)12- und cis-[B6H4(CN)2]2− sowie Kristallstruktur von Cs2[B6H5(CN)] / Preparation, 11B,13C NMR and Vibrational Spectra of the closo-Hexaborates [B6H5(CN)]2- and cis-[B6H4(CN)2]2-, and the Crystal Structure of Cs2[B6H5(CN)

By reaction of Cs2[B6H6] with in situ generated dicyanogen in aqueous alkaline solution the monocyanohydrohexaborate Cs2[B6H5(CN)] and the dicyanohydrohexaborate cis-Cs2[B6H4(CN)2] are formed. The compounds have been separated by ion exchange chromatography on diethylaminoethyl cellulose. The crystal structure of Cs2[B6H5(CN)] was determined from single crystal X-ray diffraction analysis; monoclinic, space group P21/a with a = 9.540(8), b = 9.977(3), c = 10.578(2)Å, β = 105.06(2)°. The B6 octahedron is compressed in the direction of the nearly linear B—CN bond by about 5%, with bond lengths between 1.71 and 1.76Å. The "B NMR spectra of the two compounds reveal the features of substituted B6 cages with C4v and C2v point symmetry. In the 13C NMR spectrum of Cs2[B6H5(CN)] a quartet at -139 ppm with 1J(C,B) 92 Hz is observed. The IR and Raman spectra exhibit very strong CN stretching bands for Cs2[B6H5(CN)] at 2149, and for cis-Cs2[B6H4(CN)2] at 2170 cm-1.

Reductive elimination of dimethylcarbonate from (dimethoxycarbonyl) tricarbonyl cobaltates. Isolation and crystal structures of Cs[Co(COOCH 3) 2(CO) 3] and K[(dibenzo-18-crown-6)][Co(COOCH 3) 2(CO) 3

Salts of the anion [Co(COOCH 3) 2(CO) 3] − with Cs + and K + (with the latter cation complexed by dibenzo-18-crown-6 ether) have been isolated and structurally characterized. In the trigonal bipyramidal cobaltate two C-coordinated COOCH 3 groups occupy trans-axial positions. There are ionic interactions between the cation and the terminal oxygen atoms of methoxycarbonyl involving both of the coordinated COOCH 3 groups in the case of the Cs salt but only one of them in the case of the K salt. One methoxy group of the anion [Co(COOCH 3) 2(CO) 3] − is strongly nucleophilic, as shown by the reactions with Co 2(CO) 8 or CO 2. Under an inert atmosphere [Co(COOCH 3) 2(CO) 3] − undergoes elimination of dimethylcarbonate.

The crystal structure of the cesium bronze Cs(Mo 0.95W 0.05) 7O 21

The crystal structure of Cs(Mo 0.95W 0.05) 7O 21 has been determined from a single-crystal X-ray diffraction experiment. The crystal is orthorhombic (space group Pnma), with a = 17.638(5), b = 5.448(1), c = 17.945(7)Å, and Z = 4, for a formula unit Cs(Mo 0.95W 0.05) 7O 21. The intensities ( I) of 1431 reflections, for which I > 3 σ( I), were considered observed. The structure was solved by direct and Fourier methods and refined by least squares to a value of 0.019 for the conventional R factor. It is based on the corner sharing of molybdenum coordination polyhedra, forming chains of five very distorted “octahedra” and two terminal tetrahedra. These chains, similar to those found in the structures of γ- and η-Mo 4O 11, pack to form a three-dimensional network, thus generating voids in which the Cs atoms are located with a coordination number of 12.

Crystal structure of the red cesium molybdenum bronze, Cs 0.33MoO 3

The crystal structure of Cs 0.33MoO 3 has been determined from single-crystal X-ray diffraction data. Cs 0.33MoO 3 crystallizes in space group C2 m with a = 15.862(2) Å, b = 7.728(2) Å, c = 6.4080(7) Å, β = 94.37(1)°, Z = 12, and R F = 0.033 for 1746 reflections with F 2 o ≥ 3 σ( F 2 o). The crystal is isostructural with those of the red molybdenum bronzes K 0.33MoO 3 and Tl 0.33MoO 3, but is significantly different from a crystal of the red cesium bronze Cs 0.25MoO 3. A blue powder, obtained by grinding red single crystals of Cs 00.33MoO 3, can be indexed on the basis of the cell parameters reported above.

The Chloro and Bromo Complexes of Iridium(III) and Iridium(IV). III. The Crystal-Structures of K3[IrCl6] and Cs2[IrCl5H2O] and Interpretation of the N.Q.R. Data of Chloroiridates(III)

The crystal structure of K3[IrCl6] (monoclinic, P21/c, a 1250.0, b 742.3, c 1183.3, Ir-Cl range 235.2-237.3 pm) has been redetermined , and the crystal structure of Cs2 [IrCl5H2O] [orthorhombic, C mcm , a 737.2, b 1728.3, c 801.4 pm, Ir-Cl (mean) 243.3 pm] has been determined. Results of an earlier n.q.r . Study of hexachloroiridates (111) have been interpreted on the basis of their known structures.

ChemInform Abstract: First Electride Crystal Structure.

AbstractThe crystal structure of Cs+(18‐crown‐6)2 · e‐ is determined at ‐ 57°C (space group C2/ c with Z=4).

The crystal structure of Cs 1− xLu 3F 10− x: Refinement in a higher symmetry space group

The crystal structure of Cs 1− x Lu 3F 10− x , originally described in the monoclinic space group Cm, is better described in the hexagonal space group P 6m2 . Least-squares refinement in P 6m2 has led to an improved R of 0.024, to more regular LuF distances, and to a revised composition parameter x of 0.10(1).

Behavior of M[Al2Me6N3] (M=K, Rb, Cs) with aromatic solvents and the crystal structures of Cs[Al2Me6N3]�2p-xylene and [K�dibenzo-18-crown-6] [Al2Me6N3]� 1.5(1-methylnaphthalene)

The title compounds were synthesized by the addition of AlMe3 to the corresponding azide suspended in an aromatic solvent. Both products were obtained as air-sensitive colorless crystals. Cs[Al2Me6N3]·2p-xylene crystallizes in the monoclinic space groupC2/m witha=19.143(6),b=16.227(6),c=10.392(5) A, β=114.06(2)o, and ρcalc = 1.20 g cm−3 forZ=4. Refinement led to a conventionalR value of 0.037 for 2179 observed reflections. The cesium atom resides on a mirror plane, and the anion is disordered about a twofold axis. Thep-xylene molecules sandwich the cesium ion. [K·dibenzo-18-crown-6] [AlMe6N3]·1.5(1-methylnaphthalene) crystallizes in the monoclinic space groupP21/c witha=14.176(5),b=13.021(5),c=25.324(8) A, β=98.23(4)0, and ρcalc = 1.08 g cm−3 forZ=4. The finalR value was 0.132 for 1402 observed reflections. One of the 1-methylnaphthalene molecules is disordered about a center of inversion and interacts with the potassium ion. The other solvent molecule is found roughly in layers in the lattice and also exhibits disorder of the methyl substituent. For both title compounds the AlMe3 groups of the anion exhibit a staggered (C s) conformation.

Crystal structure of Cs+[(XeOF4)3F]- and vibrational study of the oxygen-18-enriched [XeOF5]- and [(XeOF4)3F]- anions

The cesium salts of the anions (XeOF/sub 5/)/sup -/ and ((XeOF/sub 4/)/sub 3/F)/sup -/ have been prepared and characterized. The Raman spectra of Xe/sup 16/OF/sub 5//sup -/ and Xe/sup 18/OF/sub 5//sup -/ are consistent with a stereochemically active lone pair in the xenon valence shell that results in a distorted octahedral arrangement of five fluorine and one oxygen around xenon to give C/sub s/ symmetry. The X-ray structure of Cs/sup +/((XeOF/sub 4/)/sub 3/F)/sup -/ has been obtained. Crystals are cubic, space group Pa3 with a = 13.993 (7) A and Z = 8. The structure was solved by means of Patterson and Fourier synthesis and refined by the least-squares method to R = 0.0969 and R/sub w/ = 0.0960 for 355 reflections. The anion possesses C/sub 3/ symmetry and consists of octahedra of O=XeF/sub 4/E (E = lone electron pair; mean XeF = 1.90 (3) A; Xe=O = 1.70 (5) A) linked through three fluorine bridges with the trigonally bonded fluorine positioned 0.49 A above the plane defined by the three xenon atoms. The Raman spectra of the /sup 16/O//sup 18/O isotopic isomers of (XeOF/sub 4/)/sub 3/F)/sup -/ and their associated coupling patterns have been interpreted on the basis ofmore » the X-ray structure. 33 references, 6 figures, 5 tables.« less

Vibrational spectra and normal coordinate analysis of CF 3 compounds : XXXIV. The bis(trifluoromethyl)difluoroborate anion: X-ray structure of Cs[(CF 3) 2BF 2

The 10B and 11B IR and Raman spectra of the [(CF 3) 2BF 2] − anion are reported, assigned, and used to determine a quadratic local symmetry force field via a normal coordinate analysis. The crystal structure of Cs[(CF 3) 2BF 2] ( P2 1/ m, a 5.958(1), b 7.628(1), c 8.2997(9) Å, β 100.50(1)°, Z = 2, d c 2.863 g cm −3 has been determined by X-ray diffractometry. The most important force constants are f(BC) 3.68 × 10 2, f(BF) 4.17 × 10 2 and f(CF) 4.85 × 10 2 N/m, the respective mean bond lenghts being 1.618, 1.391 and 1.353 Å. The FBF and CBC bond angles are 108.1(4) and 113.6(5)°, respectively. Apparently because of Cs⋯F(B, C) interactions, one BC bond has a staggered and the other an eclipsed conformation in the solid state.

SYNTHESIS, PROPERTIES AND STRUCTURE OF TRIS(ETHYLNITROSOLATO) COMPLEXES OF MANGANESE, IRON, AND COBALT

Abstract A number of complexes derived from ethylnitrosolate (noted L−) have been prepared. Complexes of general formulas ML3 (M=Co, Fe), M ' [ML3] (M=Co, Fe, Mn; M′=N(n [sbnd] C4H9)4, P(C6 H5)4 and MPrime;[ML3] · H2O (M=Fe; M″=Rb, Cs) have been isolated. All the complexes have been characterized by IR, visible and UV spectra measurements, magnetic susceptibility and electrochemical measurements. The voltammetric behaviour shows the existence of three members series of general type ML3 n- (M=Co, Fe, Mn; n=0, 1, 2). All the solids are low-spin. Infrared data support the assumption of the same coordination structure for all the complexes. Some assignments in the IR spectra have been proposed. The crystal structure of Cs[FeL3] · H2O has been determined by single-crystal X-ray diffraction techniques using a full-matrix anisotropic least-squares program (R=0.081). Crystals are monoclinic in the space group P21 / c with cell parameters a=14.97 ± 0.01 A, b=14.07 ± 0.01 A, c=14.05 ± 0.01 A, β=94.31 ± 0.04°. The a...

Neutron and X-ray diffraction structure determination of Cs 2[VOF 4(H 2O)], a compound previously assigned Cs 2VF 6 composition

The crystal structure of Cs 2[VOF 4(H 2O)] has been studied on the basis of three-dimensional neutron and X-ray diffraction data. The structure is orthorhombic; a = 15.251(2), b = 6.486(1), and c = 7.010(1) Å; Z = 4; V = 693.46 Å 3; space group Ccmm (No. 63). From the neutron data the positions of all atomic species except vanadium were refined. The final R w value was 0.030 for 427 independent reflections with σ(I) I ⩽ 0.60 . In the X-ray case the positions of nonhydrogen atoms were refined. The final R w value was 0.022 for 509 observations with σ(I) I ⩽ 0.40 . The structure contains strongly deformed octahedral complex ions [VOF 4(H 2O)] 2−, held together by hydrogen bonds OHF (forming chains in the c direction) with cesium atoms inserted between them. The vanadyl ion VO 2+ (VO) bond distance 1.602(8) Å; X-ray value) is coordinated to four fluorine ligands and to one H 2O molecule in trans position to the vanadyl oxygen. The VF and the VO w distances are 4 × 1.919(4) and 2.268(8) Å, respectively; all are X-ray values. The OH distance is 0.987(7) Å and the HO w H angle 105.1(9)°. The coordination numbers of the two crystallographically independent cesium atoms are 13 and 11, respectively.

The crystal structure of [formula omitted

The crystal structure of Cs[VOF 3] · 1 2 H 2O has been determined and refined on the basis of three-dimensional X-ray diffractometer data (Mo Kα radiation). The structure is monoclinic, a = 7.710(2), b = 19.474(7), c = 7.216(2)Å, β = 116.75(1)°, V = 967.5Å 3, Z =8, space group Cc (No. 9). The final R and R w were 0.0295 and 0.0300, respectively, for 1356 independent reflections and 117 variables. The structure contains two crystallographically different VOF 5 octahedra linked so as to form complex chains. Two non-equivalent octahedra share one FF edge, forming V 2O 2F 8 doublets. Two F atoms, connected to different V atoms within the doublet, form an edge in the adjacent equivalent V 2O 2F 8 unit thus continuing the chain. The VO distances are 1.583(7) and 1.595(7) Å. The VF distances are in the range 1.881-2.205 Å, mean value: 1.989 Å. The H 2O group is a crystal water molecule.

Structural studies of precursor and partially oxidized conducting complexes. 19. Synthesis and crystal structure of Cs2[Pt(CN)4]Cl0.30, the first anhydrous one-dimensional tetracyanoplatinate chloride complex

Structural studies of precursor and partially oxidized conducting complexes. 19. Synthesis and crystal structure of Cs2[Pt(CN)4]Cl0.30, the first anhydrous one-dimensional tetracyanoplatinate chloride complex

Schwingungsspektrum und Kristallstruktur des fünffach-koordinierten cis-Dioxo-dipicolinato-vanadat(V)-Anions / Vibrational Spectrum and Crystal Structure of the cis-Dioxo-dipicolinato-vanadium(V) Anion

Abstract cis-Dioxo-dipicolinato-vanadate(V), Crystal Structure, IR, Raman The crystal structure of Cs[V(O)2(dipic)]·H2O (dipic = pyridine-2,6-dicarboxylate) has been determined by single crystal x-ray diffraction analysis. The compound crystallizes in the monoclinic space group P21/a, with cell constants a =737.8(3), 6=1917.5(5), c = 792.9(3) pm, β= 94.87(6)°, and Z = 4. The geometry about vanadium is a distorted trigonal bipyramid containing a cis-dioxo moiety (∢ O-V-O 109.9(3)°, V=O bond lengths 161.0(6) and 161.5(6) pm). Vibrational absorptions νs(V - 0) and νas(V=O) were found at 956 and 947 cm-1 in the IR and Raman spectrum, resp.

Crystal Structure of Cs2 [Pt(CN)4] · H2O

The crystal structure of Cs2[Pt(CN)4] · H2O has been determined from X-ray diffraction data and refined to a conventional R value of 0.068 from 2210 reflections. The compound is hexagonal, α = 9.687(2) and c = 19.336(6) A, space group C6 2-P 61, Z = 6. The given atomic coordinates represent the absolute configuration. The nearly square planar Pt(CN)42- groups form a helix with respect to the c axis. The distance between neighbouring Pt atoms in the helix is 3.543(1) A. The normal of the Pt(CN)42- group is tilted about 15 deg to the c axis leading to a considerable overlap of metal orbitals which is suggested from optical emission studies. The protons of the water molecules form hydrogen bonds to nitrogen atoms of different helices. Both Cs atoms have similar sevenfold coordination.