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A Redetermination of the Crystal Structure of Livingstonite, Hgsb4ss *

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A Redetermination of the Crystal Structure of Livingstonite, Hgsb4ss * Zeitschrift fUr Kristallographie, Bd. 141, S. 174-192 (1975) A redetermination of the crystal structure of livingstonite, HgSb4SS * By T. SRIKRISHNAN** and W. NOWACKI Department of Crystallography and Structural Sciences, University of Bern (Received 18 September 1973) Auszug Die Kristallstruktur von Livingstonit wurde neu bestimmt, urn die neue chemische Formel HgSb4Ss (statt HgSb4S7) zu bestatigen und urn die Koordina- tion von Hg und die (S-S)-Bindung in der von NnzEKI und BUERGER (1957) veroffentlichten Struktur zu studioren. Livingstonit kristallisiert monoklin mit den Gitterkonstanten a = 30,567 ::!: 0,006, b = 4,015 ::!: 0,001, c = 21,465 ::!:0,003A und f3 = 103,39 ::!:0,010, in der Raumgruppe O~,,-A 2/a mit 8 Formel. einheiten pro Zelle. Die Struktur wurde mittels Block-Diagonal-Least-Squares- Methoden bis zu einem R-Wert von 7,30/0 fur 596 beobachtete (10,20/0 fUr alle 1099) Reflexe verfeinert. Die Strukturbestimmung bestatigt die neue chemische Formel. Es kommt eine S2-Gruppe mit S-S = 2,06 A, die das zusatzliche aohte S-Atom in der neuen Formelliefert, vor. In der Struktur sind zwei Sohichtarten II c vorhanden. Die (S-S)-Bindung verknupft zwei Sb2S4-Doppelketten, wodurch zwischen ihnen eine S2-Gruppe entsteht. Die anderen Sb2S4-Doppelketten werden durch Hg-Atome untereinander verbunden. Die Bindungen zwischen diesen Doppel- ketten sind eher schwach und erklaren die perfekte Spaltbarkeit II (001). Die Koordination der Hg-Atome ist oktaedrisch; zwei der S-Atome sind stark und linear gebunden, ahnlich wie in Zinnober. In der Struktur sind vier unabhangige Sb-Atome vorhanden. Zwei davon weisen eine Viererkoordination durch S-Atome auf, in Form einer deformierten trigonalen Pyramide plus ein zusatzliches S-Atom. Die beiden anderen Sb-Atome haben eine quadratisch. pyramidale bzw. die normale trigonal-pyramidale Koordination. Die Struktur. formel von Livingstonit kann als [(Sb2S4!2 IHgII+IV] geschrieben werden [Typ IV.a! der Klassifikation von NOWACKI (1969)]. * Contribution No. 243 b; part 72 on sulfides and sulfosalts (Preliminary note: SRIKRISHNAN and NOWACKI, 1973). Present address: Center for Crystallographic Research, Roswell Park ** Memorial Institute, 666 Elmstreet, Buffalo 3, N.Y., U.S.A. A redetermination of the crystal structure of livingstonite 175 Abstract The crystal structure oflivingstonite has been redetermined with a view to confirm the new chemical formula, HgSb4Ss (not HgSb4S7) as well as to study the coordination of mercury and the S-S bond in the structure, reported by NnzEKI and BUERGER (1957). Crystals of livingstonite are monoclinic, having the cell dimensions a = 30.567 ::J::0.006, b = 4.015 ::J::0.001, c = 21.465 ::J::0.003 A and {3= 103.39 ::J::0.01°. The space-group symmetry is O~h-A 2/a and there are eight formula units in the unit cell. The structure was refined by block-diagonal least-squares method to a final R value of 7.30/0 for the 596 observed reflections (10.20/0 for all 1099 reflections). The structure confirms the new chemical formula. There is an S2 group with an S-S distance of 2.06 A, which gives raise to the additional sulfur atom in the new chemical formula. There are two kinds of layers running parallel to the c axis in the structure. The S-S bond joins two Sb2S4 double chains. The other 8b284 double chains are joined together by the Hg atoms. The bonds between these two double chains are rather weak and hence explain the presence of a perfect cleavage II (001). The coordination of the Hg atoms is octahedral; two of the 8 atoms are strongly and linearly bonded, as in cinnabar. There are four independent Sb atoms in the structure. Two of them have a coordination of four sulfur atoms which could be described as distorted trigonal pyramid plus one additional sulfur atom. The other two Sb atoms have a square pyramidal coordination and the familiar trigonal pyramidal coordination, respectively. The structural formula of livingstonite could be described as [(Sb2S4)2 IHgIIHV] [type IV.al in the classification of the sulfosalts by NOWACKI (1969)]. Introduction Livingstonite is a mercury antimony sulfide and derives its name after its discoverer, DAVID LIVINGSTONE. It is quite often found to occur along with cinnabar, which is regarded as its pseudomorph. It occurs in association with stibnite, sulfur, cinnabar and valentinite in a matrix of calcite and gypsum, at Huitzuco, Guerrero, Mexico and also at Guadalcazar, San Luis Potozi, with gypsum and sulfur (DANA, 1944). For a long time, its chemical composition was taken to be HgSb4S7, until NnzEKI and BUERGER (in 1957) gave the correct chemical composition as HgSb4Ss. Livingstonite was first investigated by RICHMOND (1936), who described it as monoclinic, belonging to the space group P 21/c. Later GORMAN(1954) reported it as triclinic. The cell dimensions reported by them are given in Table 1. NnzEKI and BUERGER (1957) investi- gated its structure and found it to be monoclinic. They also found an anomaly in the chemical composition and concluded that the correct composition is HgSb4Ss instead of HgSb4S7. Their analysis, 176 T. SRIKRISHNAN and W. NOWACKI although based on three-dimensional diffractometer data, was not very accurate, probably due to the limitations of the quality of the data and to the limitations on computing and least-squares refine- ment techniques in 1957. Quite recently, another mercury-containing sulfosalt, vrbaite, HgaTl4AssSbzSzo has been investigated in this laboratory (OHMASAand NOWACKI, 1971). We have undertaken the redetermination oflivingsto- nite to resolve the anomaly in its chemical composition with more accurate data and also to study the coordination of mercury and compare it with that of vrbaite. Experimental The crystal used for the present study was prepared from a sample of livingstonite from the type locality in Mexico. It was a thin and fibrous needle, having the dimensions 0.152 X 0.081 X 0.046 mm, with approximately cylindrical cross-section. The lattice constants were determined with the help of back- reflection Weissenberg photographs, on which the diffraction pattern of standard silicon had been superimposed to calibrate the film shrinkage. The precise cell constants determined from a least-squares Table 1. Crystallographic data oj livingstonite NnZEKI and RICHMOND GORMAN Present study (1936) (1954) BUERGER (1957) Space group P 21jc P 1 or PI A2ja A2ja a 15.14 A 7.67 A 30.25 A 30.567 ::!::0.006 A b 3.98 4.00 4.00 4.015 ::!::0.001 c 21.60 10.84 21.49 21.465 ::!::0.003 ex - 99° 12' - - fJ 104°00' 102° l' 104° 12' 103.39 ::!::0.02 y - 73° 48' - - V 2562 A3 Cell content 4 HgSb4S7 HgSb4S7 8 HgSb4SS 8 HgSb4Ss Computed density 5.06 4.89 g cm-3 Measured density 5.00 (FRONDEL) F(OOO) 3296 electrons R for observed reflections 0.19 0.073 A redetermination of the crystal structure of livingstonite 177 best fit of 20 (hOl) and 14 (Okl) reflections are given in Table 1, together with the values of NnzEKI and BUERGER (1957), GORMAN (1945) and RICHMOND (1936). The calculations were made with the help of a program written by N. D. JONES (unpublished). The crystal belongs to the monoclinic system. The systematic absences, as observed from Weissenberg photographs are hkl: k + 1 = 2n + 1 hOl: 1 = 2n + 1 (h ¥ 4n) OkO: k = 2n + 1. The possible space groups are A 2ja or Aa. But the former space group has been assumed, because an analysis of the distribution of the nor- malized structure amplitudes suggested the centric rather than the acentric space group (see Table 2). The systematic absences in hOl reflections are rather unusual. In addition to the space group extinc- tions of h = 2n + 1 and 1 = 2n + 1, there is an additional absence of h ¥ 4n. This could be only interpreted as due to the structural arrangement. There are eight formula units in the unit cell and one in the asymmetric octant. In all this we follow and confirm the 1957 analysis by NnzEKI and BUERGER. Table 2. Distribution of normalized structure factors Theoretical Experimental centric acentric <lEI> 0.657 0.798 0.886 < IE21 > 1.029 1.000 1.000 < IE2 - 11 > 1.312 0.968 0.736 lEI> 3.0 2.30;0 0.30;0 0.01% lEI> 2.0 6.90;0 5.0% 1.8 0/0 lEI> 1.0 24.4% 32.0% 36.80;0 Three-dimensional intensity data were collected by a Supper-Pace automated diffractometer having vv-eissenberg geometry and using CuK IX radiation. The intensities were corrected for Lorentz and po- larization factors. Correction for absorption was made with the help of an ICR-10 program (JOHNSON, 1963), because of the high linear absorption coefficient of the material (fl = 1068 cm-1 for CuKIX radi- ation). Z.Kristallogr. Ed. 141,3/4 12 178 T. SRIKRISHNANand W. NOWACKI Structure determination and refinement The coordinates of the Hg atoms were determined from an analysis of the Patterson synthesis. There were two big peaks In the three- Table 3. Observedand calculatedstructurefactorsfor livinystonite p p p p p p p p p p p p p p p p . , . , . , . , . , . , . , . , , _6 0 0 -8 -137 241 -240 -2 294 -258 -16 211 -182 70 81 -6 441 -440 -10 156 -142 204 11 ,6 -12 225'" 210 6 '54 -382 -, 72 -80 -17 20' -198 7 69 89 9 -220 52 8 661 667 251 94 182 87 80 160 12 24 -16 2'8 -7 79 -10 -188 -20 -7 -150 -9 59 75 12 496 -490 -20 158 -, 265 281 99 -68 -21 ,4 -. 302 10 207 _206 -12 77'4 -69 '50 -1' '2 111 '28111 111 16, 16 422 b o 24 -10 965 -982 -14 13J 126 2 8 -, -10 -121 181 '7' -11 24, -271 -15 99 85 -12 18', 195 11 -15-1' 194 _116 b 0 2 ,,4 62 1 280 138 12 61 '97 0 '58 -14 485 -459 -17 55 _1 295 '" -40 -16 -65 4 528 143 135 -420 -18 291 90 -1' 64 4H -12 69 465' -"87 -4 -18 4" -2')1_28 , -80 -14 '"
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