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Reinerite, Zng(Asoa)2T Br Trs€Rite with a Novel Type of Zn-Tehahedral

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Reinerite, Zng(Asoa)2T Br Trs€Rite with a Novel Type of Zn-Tehahedral American Mineralogist, Volume 62, pages ll29-1134, 1977 Reinerite, Zng(AsOa)2tBr trs€rite with a noveltype of Zn-tehahedral doublechainr SusRere GHose, Pe.ul BovING,WIlr-Illr A. LlCHe.psLLEAND CHr'Nc WeN Department of Geological Sciences, Uniuersity of Washington Seattle, Washington98 I 95 Abstract Reinerite,Znr(AsOs)z from Tsumeb,S. W. Africa, is orthorhombic, with cell dimensionsa = 6.092(2),b : 14.407(2),c : 7.811(l)A, space group Pbam and Z : 4. The crystal structure has been determinedby the symbolic addition method and differenceFourier synthesisand refined by the method of least squaresto an R factor of 0.051 based on 1289 reflections, measuredon an automatic single-crystaldiffractometer. The standarddeviation in Zn-O and As-O bond lengthsis 0.003 and 0.0044 and in O-Zn-O and O-As-O angles0.02". The structureof reineritecontains a new type of Zn-tetrahedraldouble chain, [ZnoOro]-, with two-tetrahedralrepeat and four-memberedrings; thesedouble chains are cross-linked into a three-dimensional framework through corner-sharing of a new type of edge-sharingZn- tetrahedraldimers and two types of trigonal pyramidal arsenitegroups. The averageZn-O bond distanceswithin the two independentZn-O tetrahedraare 1.958and 1.964A.Both the arsenitegroups have the point symmetry m, wilh averageAs-O bond distances1.776 and l.77lA and averaseO-As-O bond aneles98.4 and 96.8'. lntroduction : 2n and hol, h : 2r present. Of the two possible spacegroups, Pbam and Pba2, the first proved to be In the course of our investigation of the stereo- correct on the basisof an l(z)-test of the measured cheniistryof copper and zinc (Ghose and Wan, 1974; X-ray diffraction intensities. Ghose et al., 1974), we have now determined the A single crystal of light blue transparentreinerite crystal structure of reinerite,Zn3(AsOs)2, from Tsu- was checked for crystal perfection through a trans- meb, S.W. Africa. At Tsumeb, it occursat a depth of mission Laue photograph and then ground to a 800 m in a secondoxidation zone of the lead-zinc- sphere of diameter 0.225(2) mm. The single-crystal copper deposit, in associationwith smithsonite,hy- sphere was mounted on the syntex PT single-crystal drozincite, hemimorphite, willemite, adamite, and diffractometer,and the unit-cell dimensionswere re- olivenite(Geier and Weber, 1958).In addition to the fined by the least-squaresmethod basedon 15 reflec- configuration of the arsenitegroup, the crystal struc- tions with measured2d values between 35 and 45', ture of reineriteturned out to be of considerablein- using MoKa radiation. The cell dimensions(Table l) terest,because it contains a new type of double chain are in good agreement with those determined by consisting of corner-sharing ZnOo tetrahedra, re- Geier and Weber. All (hkl) reflections within 20 = miniscent of the amphibole-typetetrahedral silicate 65o were measured on the diffractometer by the N-0 double chains, and an edge-sharingZn-tetrahedral scan method, using MoKa radiation mono- dimer. chromatized by reflection from a graphite "single" Experimental crystal,and scintillationcounter. A variablescan rate Reinerite was reported to be orthorhombic with was used, the minimum being l"/min (50 kV, 15 possible space group Pmma by Geier and Weber mA). Out of a total of 1289reflections, 239 were less (1958). Precessionphotographs of a reineritecrystal than 3o(1), where o(1) is the standard deviation of the from Tsumeb revealedextinction conditions as0kl, k measured intensity as determined by the counting statistics. All the intensities were corrected for 1 Structural chemistry of copper and zinc minerals Part III Lorentz, polarization, and absorption factors. It29 GHOSEET AL : REINERITE Table l. Reinerite:crystal data hk I E Sign 0 16 5 3.24 e Reinerite, Znr(As0r)r: Tsuneb, S. I.i. Africa, NMNH#115409 I lr 5 2.54 f 4 | 22.53 Orthorhonbic, 'ffi c ai 6.Og2Q); Cel1 conrenr: 4[Znr(AsOa)r1 Signsand symbolsof 153reflections with E > 1.60 were determined.Out of the eight possibleE maps, b: 14.407(2) D: 4.270zcm-3 m" one showed the correct structure in terms of the ct 7.811(1) D-t 4.283 e cm-3 heavyatoms, namely 2Zn and 2 As. The symbolse,f -, -. Cell volune: 685.6(2);3 ! (MoKd) : 209 . 71 cn-1 g turned out to be +, A structure-factorcalcu- qh.^a Cr^"n. Phm lation with the heavy atoms only yieldedan R factor of 0.27. The oxygen positions were determined from a three-dimensionaldifference Fourier synthesis.The R Determinationand refinementof the structure factor at this stage was 0.21. The structure was re- A three-dimensionalPatterson synthesis was com- fined by the method of least squaresusing the pro- puted. However, due to the interactionof four heavy gram RFINE (Finger,1969), first usingisotropic and atoms, the interpretation of the Patterson map then anisotropic temperaturefactors for all atoms. proved to be difficult. The four heavy-atompositions The scatteringfactors were taken from Cromer and were determined directly by the symbolic addition Mann (1968), correctedfor anomalous dispersion method(Karle and Karle, 1966)using the computer (Cromer and Liberman, 1970).The observedstruc- program MULTAN (Germain et al., l97l). The E ture factors Fo's were weighted by l/o2(F"), where valuesfor all reflectionswere calculated. The signsof o(F.) is the standard deviation of F". A few strong the following three reflectionswith large E values low-angle reflections(e.g. 004, l2l) were strongly were chosento definethe origin: affectedby extinction. These reflectionswith Af' ) 10.0 were excludedfrom the refinement.The flnal R hk I E Sign factor is 0.051 for all (1289) reflectionsand 0.046 1922.94 + excluding l8 reflectionsaffected by extinction. The 3622.75 + shift,/errorat this stageis 0.00.The atomic positional 1772.41 and thermal parametersare listedin Table 2 and a list of observedand calculatedstructure factorsin Table In addition, the application of the ), relationship 3.'?The standarddeviations in bond lensthsand an- indicated the signs of two more reflections(0,0, l0) and (18,2,0)with E values1.90 and 1.65respectively '?To obtain a copy of Table 3, order documentAM-77-058 from to be *, *. The following three reflections were the BusinessOffice, 1909 K Street,N.W., Washington,D.C 20006. assignedsymbols: Pleaseremit $1.00in advanceior the microfiche. Table 2. Reinerite,Znr(AsO.l: atomic positionaland thermal parameters(standard deviations in parentheses) Atom R^^ Brrt R, " R. ^ Bzs zn(l) 0 0.5 0.31453 (8) 1.ro(r) L25r(r1) 99(3) 252(e) -6 (6) 00 zn(2) 0.56494(8) o.77eo8(3) 0.78434(6) 1. 04(1) 804(11) 724(2) 361(6) 2(4) -58 (8) -e (3) (1) As 0. 91312(10) 0.87 436 (4) 0.5 0. 94(r) 783(L4) 113(2) 298(8) -26(5) 00 As(2) 0.2230s(10)0.90L26(4) 0 0.97(1) 847(L5) r01 (2) 33s(8) 65(s) 00 o (1) 0 . 3304(8) 0. 0608(3) 0.5 1.34(7 ) 1304(121) 149(18) 352(59) 1s8(41) 00 o(2) 0.3349(8) 0. 2807(3) 0 1.16 (6) 1103(108) L24(16) 338(s8) 8s(38) 'oo 0(3) 0.1519(s) o.L997(2) o.3262 (4) 1.4s(5) 840(70) 2r8(L4) 534(45) s8(29) s3(s0) 162(2r) (4) o 0.0904(s) o .3965(2) 0.r736(4) 1.32(s) r372(82) 98(rr) 456(4o) -43(26) 353(s1) -42(78) xEquivalent isotropic B, calculated from anisotropic temperature factors, tForn of anisorropic tenperarure factor (x105), .*p { - i I h-.t"r|r, ) GHOSEET AL REINERITE gles as well as in thermal ellipsoidswere calculated Table 5 Reinerite,Zn,(Asor),: thermal ellipsoid parameters (standard in parentheses) using the ERROR program (Finger, personal com- deviations munication, 1972).The bond lengths and anglesare in Table 4, and the dimensionsof the thermal ahdla rol df P. with respecE to listed Arom Axls, oo *niltl'u" ellipsoidsin Table 5. The averagestandard deviation +q +b +c in Zn-O and As-O bond lengths are 0.003 and 0.088 90 90 90 0.004A, respectively,and in O-Zn-O and O-As-O r2 0.r02 89(1) r79(1) 90 angles0.02o. r3 0.153 179(1) 91(1) 90 zr(2) rL 0.r03 107(3) 79(4) 20(4) Description of the structure rz 0.r15 99(4) 161(4) 81(4) !3 0.L25 161(4) 84(4) r08(3) The crystal structure of reineriteis a three-dimen- rL 0.096 90 90 0 framework, consistingof three distinct struc- x2 0.107 71(5) 161(5) 90 sional T3 0.L23 161(4 ) ro9(4) 90 tural components: (a) dimers of edge-sharing As(2) rI o.097 114(1r) 155(11) 90 r2 0.102 90 90 r80 0.13r Ls6(2) 66(2) 90 Table 4 Reinerite,ZnlAsO.),: interatomic distances(A) and 0(1) !L 0. 104 90 90 0 angles(') (standarddeviations in parentheses) 0.108 61(105) 29(105) 90 r3 0.169 151(8) 61(8) 0 lhe Zn(1) - Tetrahedton 0(2) TL 0.102 90 90 r2 0.r07 7L2(7r) 158(71) 90 - - zn(1) - 0(1)(x2) 1.983(3) 0(1) zo(1) 0(1') 86.r(1) r3 0.149 158(r1) 68(11) 90 zn(1) - 0(4)(x2) 1.933(3) 0(1) - zn(1) - 0(a)(x2) r27,4(2) - - (1) IIean I.9s8 0(I) zn(l) 0(4')(x2) 102.9 0(3) r1 0.099 95(L2) 1,26(6) 36(4) (2) 0(4)-zn(l)-0(4') r10.6 T2 0.123 L2(9) 83(9) 79(r2) 0(1) - 0(4)(x2) 3.sr2(4) 109.5 r3 0.173 101(6) 37(8) 5s(7) 0(1) - 0(4')(x2) 3.064(4) 0(1) - 0(1') 2.709 (7 ) 0(4) TL 0.o92 74(22) 49(25) 45(32) 0(4) - 0(4') 3.179G) 0.105 114(34 ) 42 (32) Lr2(45) Mean 3.L73 r3"2 0.175 ls1 (s) 98(3) 62(4) Tl"E zn(2) - Tettahed8on zr(2) - 0(2) 1.98s(2) 0(2) - zn(2) - 0(3) 99'9(2) za(2) - 0(3) 1.953(3) 0(2) - zn(2) - 0(3') Lo9'2(2) Zn(2) - 0(3') 1.949(3) o(2) - zn(2) - o(4) 112'3(1) Zn(l)Oa tetrahedra;(b) tetrahedraldouble chains, zn(2) - 0(4) 1'966(3) 0(3) - An(2) - 0(3') 119'6(1) Zn(2)Oo tetrahedra;and Meao 1.964 0(3) - zn(2) - 0(a) 111'4(1) made up of corner-sharing 0(3') - zn(2) - 0(4) 104.s(I) (c) two isolated trigonal-pyramidal arsenitegroups, 0 (2) - 0(3) 3.016(4) Mean 109'5 0(2) - o(4) 3.284(5) As(1)O3and As(2)O,.
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