Synthesis of CsCuS[sub 6] and Cs[sub 6]Cu[sub 2](TeS[sub 3])[sub 2](S[sub 6])[sub 2] in molten Cs[sub 2]S[sub x]Te[sub y] salts. Novel compounds containing polychalcogenide ligands

Journal Article · Wed Jun 23 00:00:00 EDT 1993 · Inorganic Chemistry; (United States)

DOI:https://doi.org/10.1021/ic00065a024· OSTI ID:5847730

McCarthy, T J; Zhang, X; Kanatzidis, M C ^[1]

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1. Michigan State Univ., East Lansing (United States)

The reaction of Cu with excess Cs[sub 2]S[sub x] and Cs[sub 2]S[sub x]Te[sub y] produced two new copper/polychalcogenides CsCuS[sub 6] (1) and Cs[sub 6]Cu[sub 2](S[sub 6])[sub 2](TeS[sub 3])[sub 2] (2). Orange-red 1 was synthesized by the reaction of copper powder with Cs[sub 2]S[sub 11] in the 1.25:1 molar ratio at 270[degrees]C for 4 days. Red 2 was synthesized by the reaction of copper powder with Cs[sub 2]S[sub 6]Te[sub 0.7] in the 2:3 molar ratio at 230[degrees]C for 96 h or by the reaction of CuTe with Cs[sub 2]S[sub 6] in a 2:3 molar ratio at 250[degrees]C for 96 h. Crystal data for 1: triclinic P[bar 1], Z = 2, a = 10.664(2) [angstrom], b = 11.223(1) [angstrom], c = 7.1599(8) [angstrom], [alpha] = 94.64(1)[degrees], [beta] = 101.32(1)[degrees], [gamma] = 74.04(1)[degrees], V = 807.5(4) [angstrom][sup 3], 2[theta][sub max] = 60[degrees]. Number of data measured: 4709. Number of data having F[sub 0][sup 2] > 3[sigma](F[sub 0][sup 2]): 2800. Final R/R[sub w] = 0.036/0.044. Crystal data for 2: a = 21.072(4) [angstrom], b = 13.173(3) [angstrom], c = 11.948(2) [angstrom], V = 3317(1) [angstrom][sup 3] at 20[degrees]C, 2[theta][sub max] = 55[degrees], space group Cmca, Mo K[alpha] radiation. Number of data having F[sub 0][sup 2] > 3[sigma](F[sub 0][sup 2]): 1437. Final R/R[sub w] = 0.031/0.026. The structure of CsCuS[sub 6] is assembled from one-dimensional [Cu(S[sub 6])][sub n][sup n[minus]] centrosymmetric chains (running parallel to the crystallographic [011] direction) separated by Cs[sup +] atoms. Cs[sub 6]Cu[sub 2](S[sub 6])[sub 2](TeS[sub 3])[sub 2] contains a dimeric anion assembled from two tetrahedral Cu[sup +] atoms joined by two trigonal pyramidal TeS[sub 3][sup 2[minus]] ligands and two chelating S[sub 6][sup 2[minus]] ligands. The infrared and uv/vis/near-ir spectra of these compounds are reported. 25 refs., 6 figs., 5 tabs.

• OSTI ID: 5847730
• Journal Information: Inorganic Chemistry; (United States), Vol. 32:13; ISSN 0020-1669
• Country of Publication: United States
• Language: English

Related Subjects

37 INORGANIC
ORGANIC
PHYSICAL AND ANALYTICAL CHEMISTRY
CESIUM SULFIDES
CRYSTAL STRUCTURE
CESIUM TELLURIDES
COPPER SULFIDES
COPPER TELLURIDES
ABSORPTION SPECTROSCOPY
CHELATES
CHELATING AGENTS
CHEMICAL PREPARATION
LATTICE PARAMETERS
LIGANDS
MILLER INDICES
MOLTEN SALTS
STOICHIOMETRY
TRICLINIC LATTICES
X-RAY DIFFRACTION
ALKALI METAL COMPOUNDS
CESIUM COMPOUNDS
CHALCOGENIDES
COHERENT SCATTERING
COMPLEXES
COPPER COMPOUNDS
CRYSTAL LATTICES
DIFFRACTION
SALTS
SCATTERING
SPECTROSCOPY
SULFIDES
SULFUR COMPOUNDS
SYNTHESIS
TELLURIDES
TELLURIUM COMPOUNDS
TRANSITION ELEMENT COMPOUNDS
400201* - Chemical & Physicochemical Properties