Hodrushite—a new sulphosalt

1970 ◽  
Vol 37 (290) ◽  
pp. 641-648 ◽  
Author(s):  
M. Koděra ◽  
V. Kupčík ◽  
E. Makovický

SummaryHodrushite, a new sulphosalt of copper and bismuth, was found in the Rosalia ore vein at Banská Hodrušá near Banská Štiavnica, Czechoslovakia. It has chemical composition Cu8·12Bi11·54Fe0·29S22 (as determined by electron-microprobe method) close to Cu8Bi12S22. Symmetry is monoclinic, space group A2/m, lattice constants a 27·21, b 3·93, c 17·58 Å, β 92° 9′, measured density 6·35, calculated density 6·45 g/cm3. Microhardness 200 kg/mm2, anisotropic, weak bireflectance, creamy with pinkish tint, maximum reflectivity about 6000 Å. Crystals needle-shaped and striated along [010], colour steel-grey, quickly tarnishing to bronze. Associated with quartz, hematite, and chalcopyrite. Closely related to cuprobismutite.

1990 ◽  
Vol 45 (8) ◽  
pp. 1118-1122 ◽  
Author(s):  
R. J. Schubert ◽  
K.-J. Range

Single crystals of (n-C4H9)4NAu(CN)2 were obtained by crystallization using the temperature decreasing method in a newly developed computer-controlled apparatus. The colourless crystals are monoclinic, space group A2/n, with a = 20.216(2) Å, b = 13.130(1) Å, c = 9.328(1) Å, and β = 109.69(1)°. The measured density is 1.45 g/cm3, which agrees with the calculated density of 1.40 g/cm3 for Ζ = 4. The structure was solved by Direct Methods using 674 independent reflections and refined by least-squares procedures to conventional and weighted R factors of 0.068 and 0.058, respectively. The nearly linear [Au(CN)2]--anions form pseudohexagonal layers, in which they are arranged parallel to each other. The shortest Au—Au distance is 8.05 A. The stacking of the layers produces pseudo-trigonal channels, occupied by the cations. The tetra-n-butylammonium cation has four ordered trans chains with idealized D2d symmetry (4̄2 m).


1988 ◽  
Vol 43 (10) ◽  
pp. 1219-1223 ◽  
Author(s):  
Johannes Beck

PPh3Au(tolN5tol) is obtained by the reaction of PPh3Au+ClO4- with Tl(tolN5tol). It crystallizes in the monoclinic space group P21/c with the lattice parameters a = 1548.8(5), b = 1070.7(2), c = 1779.1(3) pm, β = 90.33(2)°, Z = 4. In the monomeric complex the gold atom is nearly linearcoordinated by the phosphorus atom of the PPh3 group and nitrogen atom N3 of the pentaazadienido ligand ( N3 - Au - P 178.4°). tolNN(NCH3)NNtol crystallizes in the orthorhombic space group Pccn with the lattice constants a = 2426.7(9), b = 469.3(2), c = 1195.3(4) pm. The unit cell contains four molecules, located on twofold axes. Due to the isolobality of the CH3 and the PPh3Au group, the two structures are closely related. Both contain the typical planar zig-zag chain of five nitrogen atoms with located double bonds N1-N2 and N4 - N5 (from 119.8 to 126.6 pm) and shortened single bonds N2 - N3 and N3 - N4 (132.7 to 140.0 pm).


1985 ◽  
Vol 40 (1) ◽  
pp. 13-18 ◽  
Author(s):  
Kay Jansen ◽  
Kurt Dehnicke ◽  
Dieter Fenske

The syntheses and IR spectra of the complexes [Mo2(O2C-Ph)4X2]2⊖ with X = N3, CI, Br and the counter ion PPh4⊕ are reported. The azido and the bromo complexes are obtained from a solution of [Mo2(O2CPh)4] with PPh4N3 in pyridine or by reaction with PPh4Br in CH2Br2, respectively. When (PPh4)2[Mo2(O2CPh)4(N3)2] is dissolved in CH2Cl2, nitrogen is evolved and the complex with X = CI is obtained. The crystal structure of (PPh4)2[Mo2(O2CPh)4Cl2] · 2CH2Cl2 was determined from X-ray diffraction data (5676 observed independent reflexions, R = 0.042). It crystallizes in the monoclinic space group P21/n with four formula units per unit cell; the lattice constants are a = 1549, b = 1400, c = 1648 pm, β = 94.6°. The centrosymmetric [Mo2(O2CPh)4Cl2]2⊖ ion has a rather short Mo-Mo bond of 213 pm, whereas the MoCl bonds are very long (288 pm)


1994 ◽  
Vol 49 (12) ◽  
pp. 1763-1773 ◽  
Author(s):  
Jochen Ellermann ◽  
Jörg Sutter ◽  
Falk A. Knoch ◽  
Matthias Moll ◽  
Walter Bauer

Reaction of (1) in CH2Cl2 with benzimidazole yields . The salt [4]+BPh4- has been prepared in THF by metathesis of [4]+Cl- with NaBPh4. Deprotonation of the cationic ring in [4]+BPh4- was accomplished using 1,8-diazabicyclo[5.4.01,7]undec-7-ene and resulted in the six-membered carbacyclophosphazene (6). Treating 1 with 8 -hydroxyquinoline in CH2Cl2 yields the octahedral cis-complex = 8-oxyquinolinate group). The com pounds [4]+BPh4-, 6 and 7 are characterized by their IR, Raman, 31P{1H} NMR, 13C{1H} NMR, 1H NMR and mass spectra. Crystals suitable for X-ray structure analyses have been obtained for [4]+BPh4- and 7×0.5 CH2Cl2. The colourless plates of [4]+BPh4- crystallize in the triclinic space group P1̄, with the lattice constants a = 1172.7(3), b = 1326.2(3), c = 1806.1(6) pm; α = 100.79(2), β = 103.71(3), γ = 108.18(2)°. The black blocks of 7×0.5 CH2Cl2 crystallize in the monoclinic space group P 21/c with the lattice constants a = 1159.0(10), b = 2008.9(10), c = 2034.6(12) pm; β = 105.86(5)°.


1994 ◽  
Vol 49 (4) ◽  
pp. 489-493 ◽  
Author(s):  
C. Müller ◽  
P. Böttcher

The reaction of trimethylamine, H2S, and sulfur in ethanol yields orange crystals of bis(trimethylammonium) hexasulfide. The com pound crystallizes in the centrosymmetric monoclinic space group P 2/c. The lattice constants are a = 10.310(7), b = 5.752(2), c = 13.348(10) Å, β = 98.41(6)°. The S26-chain has a helical all-trans-conformation (sequence of the signs of torsion angles +++ and --- ).


1993 ◽  
Vol 48 (7) ◽  
pp. 1009-1012 ◽  
Author(s):  
Kurt Merzweiler ◽  
Harald Kraus

[{Cp(CO)2Fe}SnCl3] reacts with Na2Se in THF to form the compound [{Cp(CO)2Fe}3ClSn3Se4] 1. 1 crystallizes in the monoclinic space group P21/n with 4 formula units per unit cell. The lattice constants are α = 1435.2(7), b = 1124.4(4), c = 1972.7(12) pm, β = 94.59(4)°. According to the X-ray structure determination 1 contains a bicyclic Sn3Se4 framework.


1989 ◽  
Vol 44 (8) ◽  
pp. 884-888 ◽  
Author(s):  
Dieter Fenske ◽  
Kurt Merzweiler

The chiral diphosphine 1 reacts with [(diolefin)Rh(THF)2]PF6 (diolefine: 1.5-cyclooctadiene, norbornadiene) to form the complexes 4 and 5. The structure of 4 was determined by single crystal X-ray analysis. 4 crystallizes in the monoclinic space group P21. The lattice constants (at 180 K) are: a = 974.0(6); b = 3889.2(29); c = 1309.4(5) pm; β = 105.25(4)°. The hydrogenation of methyl-α-acetamidocinnamate in the presence of 5 yields (R)-N-acetylphenylalanine methyl ester with 33% enantiomeric excess.


2016 ◽  
Vol 80 (7) ◽  
pp. 1265-1272 ◽  
Author(s):  
Anthony R. Kampf ◽  
Barbara P. Nash ◽  
Maurizio Dini ◽  
Arturo Molina A. Donoso

AbstractThe new mineral gajardoite (IMA2015-040), KCa0.5As3+4O6Cl2·5H2O, was found at the Torrecillas mine, Iquique Province, Chile, where it occurs as a secondary alteration phase in association with native arsenic, arsenolite,chongite, talmessite and torrecillasite. Gajardoite occurs as hexagonal plates up to ∼100 μm in diameter and 5 μm thick, in rosette-like subparallel intergrowths. Crystals are transparent, with vitreous lustre and white streak. The Mohs hardness is ∼1½, tenacity is brittleand fracture is irregular. Cleavage is perfect on {001}. The measured density is 2.64 g/cm3 and the calculated density is 2.676 g/cm3. Optically, gajardoite is uniaxial (–) with ω = 1.780(3) and ε = 1.570(5) (measured in white light). The mineral is very slowly soluble in H2O and slowly soluble in dilute HCl at room temperature. The empirical formula, determined from electron-microprobe analyses, is (K0.77Ca0.71Na0.05Mg0.05)∑1.58As4O11Cl1.96H9.62.Gajardoite is hexagonal, P6/mmm, a = 5.2558(8), c = 15.9666(18) Å, V = 381.96(13) Å3 and Z = 1. The eight strongest powder X-ray diffraction lines are [dobs Å(I)(hkl)]: 16.00(100)(001), 5.31(48)(003),3.466 (31)(103), 3.013(44)(104), 2.624(51)(006,110,111), 2.353(36)(113), 1.8647(21)(116,205) and 1.4605(17) (119,303,216). The structure, refined to R1 = 3.49% for 169 Fo > 4σF reflections, contains two types of layers. One layer of formulaKAs3+4O6Cl2 consists of two neutral As2O3 sheets, between which are K+ cations and on the outside of which are Cl– anions. This layer is topologically identical to a slice of the lucabindiite structureand similar to a slice of the torrecillasite structure. The second layer consists of an edge-sharing sheet of Ca(H2O)6 trigonal pyramids with isolated H2O groups centred in the hexagonal cavities in the sheet.


1985 ◽  
Vol 40 (7) ◽  
pp. 861-863 ◽  
Author(s):  
Ulf Thewalt ◽  
Maria Burger ◽  
Regina Mausser ◽  
Konrad Holl

Abstract S4N4 reacts with NH4+FeBr4- in benzene to give the 1:1 inclusion compound NH4+FeBr4- • S4N4. The dark red crystals are monoclinic, space group Cc with Z = 4 and lattice constants a = 6.430(1), b = 17.644(4), c = 12.180(2) Å , and β = 90.77(3)°. An X-ray analysis shows that the geometry of the S4N4 group is almost identical to that of crystalline tetrasulfur tetranitride. The S4N4 molecule is surrounded by ionic neigbors in such a way that the S atoms form close contacts to Br atoms of the FeBr4- anions and the N atoms are close to the NH4+ cations.


2020 ◽  
Vol 58 (4) ◽  
pp. 533-542
Author(s):  
Anthony R. Kampf ◽  
Robert M. Housley ◽  
George R. Rossman

ABSTRACT Northstarite, Pb6(Te4+O3)5(S2O3), is a new mineral from the North Star mine, Tintic district, Juab County, Utah, USA. It is an oxidation-zone mineral occuring in a vug in massive quartz-baryte-enargite-pyrite in association with anglesite, azurite, chrysocolla, fluorapatite, plumbogummite, tellurite, zincospiroffite, and the new mineral adanite. Crystals are beige short prisms with pyramidal terminations, up to about 1 mm in length. The mineral is transparent to translucent with adamantine luster, white streak, Mohs hardness 2, brittle tenacity, irregular fracture, and no cleavage. The calculated density is 6.888 g/cm3. Northstarite is uniaxial (–) and nonpleochroic. The Raman spectrum is consistent with the presence of tellurite and thiosulfate groups and the absence of OH and H2O. Electron-microprobe analyses gave the empirical formula Pb5.80Sb3+0.05Te4+5.04S6+1.02S2–1.02O18. The mineral is hexagonal, space group P63, with a = 10.2495(5), c = 11.6677(8) Å, V = 1061.50(13) Å3, and Z = 2. The five strongest X-ray powder diffraction lines are [dobs Å(I)(hkl)]: 3.098(100)(113), 2.957(88)(300), 2.140(42)(223), 1.7335(41)(413), and 1.6256(31)(306). The structure (R1 = 0.033 for 1476 I > 2σI reflections) is a framework constructed of short (strong) Pb–O and Te–O bonds with channels along the 63 axes. The thiosulfate groups at the centers of the channels are only weakly bonded to the framework.


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