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Crystal Structure, Hydrogen Bonding and Relations with Haidingerite And American Mineralogist, Volume 64, pages 1248-1254, 1979 Krautite, Mn(HTOXAsOTOH):crystal structure, hydrogenbonding and relations with haidingeriteand pharmacolite MICHELE Cern .a.No MnRnnLLa FnINcHINI-ANGELA Istituto di Mineralogia, Cristallografia e Geochimica "G. Spezia" Universitd di Torino, Via S. Massimo 22, 10123 Torino, Italy Abstract The crystal structure of synthetic krautite was solved (direct methods) and refined isotrop- ically (R:0.112) in spacegroup P2, with2294 reflectionsmeasured on a single-crystaldif- fractometer,with MoKc radiation. The unit-cell parametersate: a :8.012(2), b: 15.956@, c : 6.801(2)A,P : 96.60(3)";Z :8. A strong F2r/n pseudosymmetryappears in the struc- ture, yet the averagepseudo-center is slightly shifted from the correct position l/4,0, l/4 n spacegroup Y2r/n."Ihe structureis built up by (010)layers of AsO_oand MnOu coordination polyhedra.In eachlayer, MnOu octahedrashare edges to form [0Tl chahs, which sandwich the AsOotetrahedra. Adjacent layers are related by the screwaxis and are linked by four out of twelve independenthydrogen bonds; two of them are acidic and two are donatedby water molecules. One of the latter hydrogen bonds is probably bifurcated, since the water molecule is involved in two contacts2.92arLd 3.08A long. Haidingerite (CaHAsOo'HrO) and pharma- colite (CaHAsOo. 2HzO) show similar structuresformed by layersof coordination polyhedra connectedby hydrogenbonds. For 11e5ingle-layer topology, krautite resemblespharmacolite (chain-like structure) more than haidingerite (network-like structure), since the increase of coordination number from Mn2* to Ca2* is compensatedby the increaseof water content. Introduction strong mica-tke (010) cleavages,so that analogous structure types seemappropriate, in spite of In a seriesof structural and crystal-chemicalinves- layered the fact that the symmetries are different (rronoclinic tigations on mineral arsenatescontaining hydrogen for krautite and orthorhombic for haidingerite), and bonds (Catti et al., 1977), the manganesearsenate important differences appear in their X-ray powder krautite, recently described and characterized as a patterns. new mineral by Fontan et al. (1975),has been exam- ined. The other known natural manganesearsenates Experimental are a large group of basic arsenates(Moore, 1967), manganesehoernesite (Mn, Mg)r(AsOo)r' 8HrO, and Since good quality single crystals could not be the new mineral CaMn(HAsO)r'ZIJ.,O (Permingeat found in the natural samplesof krautite (Fontan et et al., in preparation). The synthetic crystalline al., 1975),synthetic crystalline MnHAsOo' HrO was phases reported in the system MnO-As'Or-HrO prepared. By mixing aqueoussolutions of MnCL and (Pascal,1966, p. 923) are Mnr(AsOo),'HrO, KHrAsOo a transparent gel was obtained (Deiss, MnHAsOo' HrO, Mn(HrAsOo)', Mn(HrAsOn)t l9l4), from which many small pink balls (about 2 .3H"O, and MnHAsOo'4HrO; the last compound mm diameter) precipitated;each ball was formed by is probably isomorphous with brassite, MgHAsOn tiny, crystalline packets of MnHAsOo'H'O. Every .4H2O, the structure of which is known (Protas packet contained very thin {010} lamellae,with fre- and Gindt, 1976). Krautite is the first acid man- quent polysynthetic twinning. With great difficulty ganousarsenate studied structurally; we aim to clar- an irregular crystalline fragment 0.30 x 0.10 x 0.02 ify the crystal-chemical relationships with its calcium mm could be isolated,and was usedfor all measure- homolog haidingerite, CaHAsOo'HrO (Cassien et ments. al., 1966:'Calleri and Ferraris, 1967).Indeed, both By meansof Weissenbergphotographs and single- minerals show very similar cell parameters and crystal diffractometry the monoclinic unit cell offi3-{oax / 79 / I I l 2- l 248$02.00 1248 CATTI AND FRANCHINI-ANGEL/I: KRAUTITE 1249 reported by Fontan et al. was confirmed. The least- Table l. Atomic fractional coordinates and thermal parameters squaresrefinement of 25 0 valuesmeasured on a dif- (A'?) fractometer [tr(MoKa) : 0.71069A]yielded the unit- cell parameters a : 8.012(2), b : 15.956(4),c : 6.801(2)4,B :96.60(3)". Othercrystal data are:V : 863.7A',Z:8, M :212.879,p (meas): 3.30g cm-, Mn(1) 0.4033(4)1' 0.0451(z) 0 .6520\4) 0 .69(4) : Mn(l') 0 . I 069(4) -0 .0455(2 ) 0.9043(4) 0.16\41 (Fontan et al.,1975),p (calc) 3.274g cf,-', f(000) Mn(2) 0.8581 (4) 0 .0663(2) 0.r631(4) 0.71(4) : I128,p(MoKc) : .l I1.7 cm-'. On the basisof sys- I"ln(2') o.65ll(4) -0.0661(2) 0 .393414) o .70(4) tematic absences,the spacegroup could be either p2, As(1) o,4087\Z) 0 .0874(r ) 0.1473(3) 0.61(3) or FZ,/m; an analysis of statistical tests on the dif- As(l') o. l ooo(2) -0.0881(1) 0.4075(3) 0.57(3) As(z) 0.8140(2) 0.r014(r) 0.6689(3) 0.52(3) fraction intensities to detect the symmetry center As(2') o.6976\2) -0.r035(r) 0.8891(3) 0.52(3) gave ambiguousresults. o(l ) o.297 (z) 0.17r(r) o.zoz\z) r.l(2) The intensities were measuredon a Philips PW o(t') 0.zlrlz) -0.r69(1) 0.35r(2) 1.1(2) -o ll00 automatic four-circle diffractometer with the o(2) o.329\2) 0 .036(I ) .054\zl o.7(z) o(2') o. r 83(2) -0 .036(r ) o.612\21 1.o(z) following conditions: MoKa radiation, graphite o(3) o.449\ZJ 0.023(r) o.342\ZJ 0.9(2) monochromator,0 = 30", o, scan,A<.r : 1.40o,scan- o(3') 0.058(1) -0 .022(I ) o.zr4\z) 0.3(z) ning o(4) 0.603(z) 0 129(1) o.092\?.\ r.3(2) speed0.04o s-', backgroundtime 5 secon both oi4') -0 .()90(z) -o.r29(r) 0.462(2) O.7\Z) sidesof each peak, attenuatingfilter inserted for in- o( 5) 0.624121 0.134(1) o.1r7(zl 1.1(2) tensitieshigher than 60000counts s-', three reference o(5') 0.888(2) -0.133(r) 0.84r(z) o.7lz) reflections.By removing the reflectionswith = o(6) 0.916(z) 0 .050{I ) 0.862(2) o.7(z) l.F"l o(6') 0.593\Z) -0.0510) o.696(2) o.9(2) 3o(lF"l),2294 independentobservations remained for o(7) 0.808(2) o .044(l ) 0.462(z) 1.0(2) this study.' o(7') 0.1 07 (zl -0 .045(r ) | .097(2) 0.9(2) o(8) 0.938(z) 0.189(1) o.644(2) l .4(2) Solution and refinementof the structure o(8') 0.583(Z) -0.190(r) o.922(3) I .6(3) w(r) 0.264lz) 0.164(l) 0.583(2) r.5(2) The program MulreN based on direct methods w(l') o.248\2) -0.166(1) 0.964(2) r.4lz) (Germain et al., l97l) was usedto solvethe structure. w(2) o.960\2) 0.r90(r) 0.168(3) r.8(3) \4(2') o,545\2) -0.187( l ) 0.391(3) 1.8(3) In the centrosymmetricalspace group Y2,/m only pseudo-solutionswere obtained; the correct solution Estimated standard deviations are given in Parentheses and refer was found in the non-centrosymmetricalspace group to the last decimal place. P2,, showing the positions of the four As and four Mn independentatoms. By subsequentstructure-fac- tor calculationsand Fourier differencemaps, all the severalatoms becamenon-positive-definite. No ab- oxygen atoms were located. The full-matrix least- sorption correction could be performed,owing to the squaresrefinement with isotropictemperature factors irregularity of the crystalline fragment; this must for all atoms converged : to R 0.112;anomalous have introduced large systematicerrors into the data, scatteringof As and Mn atoms was correctedfor. and becauseof the lamellar shape of the crystal and of y the coordinate of As(l)'z was locked during the re- the large value of the linear absorption coefficient, finement to fix the origin. The following weighting and would account for the failure of the anisotropic schemewas used: w: l/(5 x lO-4l,ql,+ l); then the refinement. Table I reports the final atomic frac- averagevalues groups of 42 for of reflections were tional coordinates;large values of the e.s.d.'scan be practically constant.An anisotropic refinement was observedand could be ascribedto the pseudo-sym- tried unsuccessfully, since the temperature factors of metry of the structure (cf. the discussion), which causesa high correlation between atomic positional I To receive a copy of the structure factor table, order parameters in the refinement. Document AM-79-ll3 from the BusinessOffice, Mineralogical Society of America, 2000 Florida Avenue, NW, Washington, D. Discussion C. 20009.Please remit $1.00in advancefor the microfiche. 2 A single figure in parentheses denotes an atom of the Pseudo-symmetryand descriptionof the structare asymmetric unit; primed figures mean the pseudo-symmetry A strong PZ,/n pseudo-symmetryis shown by in- operation l/2 - x, r, | /2 - z. The secondfigure 2 is included for atoms in the equivalent position 7, l/2 + y, Z Roman numerals spection of Table l. All atoms can be grouped in representthe following translations:I, -c; II, +c; III, -a; IV, +a; pairs related by a pseudo-centerof inversion, which - V, +a b + c; VI, +r + c; VII, +2a + c. is located on the averageat x : 0.2555,! : O, 2 : 1250 CATTI AND FRANCHINI-ANGEI.A: KRAUTITE 'table 2. Interatomic distances and O-As-O angles in the four Table 3. Interatomic distances and O-Mn-O angles in the Mn independent AsOa groups coordination Polyhedra Mn(I')- o(Z'i 2.r5(r)i As(l)- o(l) l .67(2) A As(l')- o(1') t.64\2)A Mn(l) o(Z)II 2.15(r)A - - As(1.) o(2) r.65(r) As(lr) o(2') r.69(r) Nln(l)- o(3) z.2l(l) Mn(1')- o(3')II z.zz\t ) As(l) - o(3) L67(l ) As(1')_ o(3r) r.69(t) Mn(1 ') o(2)II z.zo(r) As(l) - o(4) r.7'7(Z) As(l')- o(4r) r.73(r) Mn(I ) O(2') 2.18(l ) '1 Aver a8e t.69 Average I .69 N{n(1)- O(5) 2.28\Z) ,,n11 - ois')III z,24\r ) z.l5(1) tr{,(1,)- 6161III z.r6(l) es(z) o(5) I .68(2) As(2')- o(5') r.66(l) Nln(l)- o(6') Asiz)- o(6) L 68(1) As(2')- 0(6') i.700) Mn(r) w(1) 2,22t2) Mn(1')- w(1') z.z4\z) As(2)- O{7) I .68(2) As(2')- o(7') 1.69U ) AVera gc z.z0 Average z.z0 As(2)- o(8) | .'t3\z) As(2')- O(8') 1.69(2) Average 1,69 Average I .69 .IV Mn(Z)- O(4) z.z1\z) f4n(2') O(4') 2,30(l) o(r)...o(z)2,?9A t14.3" o(1,)...o(2')2.79A 114,0" - ou).
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