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Download the Scanned American Mineralogist, Volume 64, pages 1243-1247, 1979 Senegalite, AI2(OH)3(H,O)(PO.), a novel structure type Tenny D. KEEGAN, TaKAHaRU ARAKr AND PAUL B. Moonn Department of the Geophysical Sciences, The University of Chicago Chicago, Illinois 60637 Abstract Senegalite,AIr(OH)'(HTOXPO.), Z : 4, orthorhombic, spacegrovp Y2rnb, a : 7.675(4), b : 9.711(), c : 7.635(4)A, is a new structure type based on chains of composition | [slAlt6lAl(OH)r(HrO)(Op).]or f,[t5t41tot41f*]where @is a coordinating oxygen and Op is phosphateoxygen. R:0.024 for 1288independent reflections. Two symmetry-equivalentchains run parallel to [01] and [T0U, each basedon distorted A(OH)3(HrO)(Op), octahedraland Al(OH)r(Op), trigonal bipyramidal edge-sharingdimers which further corner-link to completethe chain. Corner-linking eot tetrahedraknit neigh- boring chains to form an open sheet parallel to (010). Further tetrahedral corner-links to chainsrelated by the D-axialglide form an open polyhedralframework structure. Hydrogenbonds including OH ... OW, OH ... O and OW ... O rangingfrom2.'73 to 3.24A areproposed. Bond-distance averages arer5rAl(l)-O : 1.848A,t6lAl(2)-O : 1.899A,andtalP- O: 1.5344. Introduction a small effect. Symmetry-equivalent reflection pairs Senegalite, a new and relatively uncommon min- were then averaged, and after applying Lorentz and eral, was first described by Johan (1976). He reported polarization corrections, 1288 independent F" were details are summarized in the composition AlrPOo(OH)..HrO, based on chem- obtained. Experimental ical analyses of material from the type locality at the Table l. Komondiako Iron Mine (magnetite ore) in the Fa- Solution and refinement of the structure l€me River Basin of east Senegal, Africa. It occurs in the oxidation zone of the deposit, associated with tur- A three-dimensional Patterson map P(u, v, w) al- quoise, augelite, wavellite, and crandallite. Our in- lowed derivation of three independent atomic posi- vestigation was undertaken to determine the crystal tions assumed to be Al and P atoms, which consti- structure, ascertain the role of water in the species, tuted the basis of the weighted B-general synthesis and discern the relationship of this mineral to other (Ramachandran and Srinivasan, 1970, p. 96-119). phosphate hydrate structures involving Al3*. All independent atomic positions excepting hydro- gens thus obtained were then applied to full-matrix Experimental section least-squares refinement, the first two cycles with iso- A single crystal was obtained from a type-locality tropic temperature factors and the subsequent four specimen, provided by the Mineralogical Research cycles with anisotropic thermal parameters. The final Company of San Jose, California. All parameters refinement converged to R : 0.024 and R- : 0.038, were redetermined utilizing calibrated precession where photographs, yielding the results in Table l. Ex- - - P:- >ll4l l4ll anrr p -: [xl4l l4l)'l'" tinction criteria, in agreement with the earlier study, ^ p1p"; .rru '-" >.lr.r hemimorphic development of the crystals, and the I I success of the structure refinement established the with w : o-' of ,F". Refinement minimized w(F" - acentric groap F2rnb. Careful measurement of the F")'. crystal and application of the Gaussian integral Scattering curves for Al'*, Po and O- were ob- method (Burnham, 1966) permitted application of tained from Ibers and Hamilton (1974, p. 149), and absorption correction which, owing to low linear ab- anomalous dispersion corrections, Lf ", for Al and P sorption coefficient and favorable crystal shape, was from Cromer and Liberman (1970). Positions of hy- 0003_004){/ 7 9/ | | l2-1243$U.00 1243 t244 KEEGAN ET AL.: SENEGALITE Table l. Experimental details for senegalite Table 2. Senegalite. Atomic coordinate parameters f (A) Crystat Cell Data Aton a, A 7.675(4) b, ^ s.7rt(4) A1(r) \ 0.1e887(7) o.s22s (1) c, A 7 635(4) A1(2) 0.8832(1) 0. 34948(8) 0.6620(r) Space group P2rltb P 0.sr93(1) 0.482s2(6) 0.6868 7 (8) Fomula A1, (0H) 3(H2C) (P04) o(1) o.7t7s(3) 0 .4818 (2) 0.7206(3) o(2) 0.43rr(3) (2) 0 (3) (B) 0.s6rs .837s IntensityMeasurments 0(3) 0.446s(3) 0.3349(2) 0.6882 (3) (2) 0.37(lid), 0.104(llb), 0.28(llc) o(4) 0.484s(3) o.sso2 0.sI16(3) Rotation axis a[100] Max (sine)/l 0.80 0H(r) o.72ss(3) o.2ss2(2) 0.s134(3) Scan speed, deg per nin 1.0 0H(2) 0.0423(3) 0.42s4(2) 0.8294(2) Base scan width, deg 3.2, widening to 6 8 at higher 1eve1s oH(3) 0.83r0(3) 0.24s2(2) 0.8698(2) Background counts Stationary, 20 s at beinning and end of scan Reciprocal space coverage hk9. and hkQ. with ll = 0-11 Radiation MoKor (l 0.7093 A), graphite nonochionator ol1l 0. 0521(3) 0.2018 (2) 0.60s0 (3 ) TndFhFhianr F- 1288 tEstinatecl standard enors in parentheses refer to the last disit . (C) Absorption Correction u, cn-' 8 11 tancesand angles,Table 4 the anisotropicthermal vi- Gaussian integrol inteflal 7 Ttansnission factor range 0 857-0.925 bration parameters,Table 5 the parametersfor the ellipsoidsof vibration, and Table 6r the structurefac- drogen atoms were sought on difference Fourier tors. maps after final refinement,but residual peaks were rTo a copy of Table 6, order Document AM-79-lll interpretedfor OH(l) and OH(2), the othersremain- obtain from the BusinessOffice, Mineralogical Societyof America, 2000 ing ambiguous.Table 2 presentsthe refined atomic Florida Avenue, N.W., Washington, D. C. 20009.Please remit coordinates,Table 3 the polyhedral interatomic dis- $ | .00in advancefor the microfiche. Table 3. Senegalite. Bond distances and angles t A1(r) A1(2) P m 6r;-o621 t1) t.788(2) Ar(2)-o(4)(2) r.B2o(z) P-o(4) I.sr4(2) Ar(r) -oH(1) 1.8r6(2) Ar(2) -o(r) 1.860(2) P-o(2) 1.s39(2) (3) A1lr;-onJs; 7.828 (2) Ar(2)-oH(1) r.8ss(2) P-o(3) 1.s3s(2) A1(1 ) -0 (3) 7.872(2) A1(2) -oH(2) 1.91s(2) P-o(1) 1.s46(2) (3) A1(1)-oH(2) I .93s(2) Ar(2)-oH(3) r.s24(2) average I .534 average 1.848A A1(2) -ol\' r . e8r(2) O-P-O'angles (') average 1.899 apica I - equatori al 0-{r-4 (.) o (2)-0 (3) 2.48r(3) 107.4(1) (3)-6116r, oHlz; {s) 2.406 (3) * 7s.4(7) o(1)-o(4) 2.48s(3) 108.8(1) o(3) -oH(r) 2.63s(3) 91.3 (1) oH(2)-oH(3) 2.406(s)* 77.6(r) o(1)-o(2) 2.498(3) r08.2(1) (3) (2) oH(1) -or112; 2.6s r (3) 8s.e(r) o(4) -olll 2.620(3) 87.0(1) 0(3)-o(4) 2.sos(3) r10.3(r) (1)-o(s) otz) 2.66s(3) e3.4(r) oU)Q) -rxe) 2.6s2(3) e0.4 (r) 0 (2)-0 (4) 2.s24(3) lrr .s (r) (1)-6",r,(s) o6zy 2.68s(3) 92.2(1) @(l)-ow 2.6s4(3) 86.4 (1) 0(r)-0(3) 2.s26(3) 1r0.6(r) (3) o(3) -0H13; 2.702(3) s3.8(r) oH(3)-OW 2.673(3) 86.4(r) average 2.5O4 109.5 average 2.625A 90.0 0(1)-oH(2) 2.681(3) s0.s (r) Hydrogen bonds o(1)-0H(3) 2.707(3) 91.3 (r) equatorial o(1)-oH(r) 2.770(3) s2.4O,) ouJz1...tow(l) 2.731(3) (1)-q11r; (3) (2) (1) o6z1 3.018 (3) r13.r(r) o(r)-o(4) 2.72s(3) ss.s(1) oHisl " 't661; 2.789(3') (1) (2) oqzl -oH6ry 3.1s3(3) r22. o (7) o(+)(2)-on(r) 2.7s0(s) es.s(1) ol|I(1)...>oH(3) 2.840(s) (3) (2)...to,r, on611 -oH 1s; 3.220(3) r24.t(t') oH(2) -olll 2.767(3) 90.s(1) oH1rl tt) 3.tsz(3) aveTage 3.130 LLg.7 oH(1)-ofr(3) 2.84r(3) s6.1(1) ow(I)...ro(z) 3.242 (3) average 2.682 90.0 api ca I Angles with 0l'I (3) (r) o {sy -oH 621 772.s(L) onqz; -ow -o 121 10s. 7(r) (2) oH(z)-ow(r) -611 Js; 10s.7(1) (2) olzy-ow(1) -6s131 r22.2(L) fEstinated standard errors refer to the last digit. The equivalent positions (referred to Table 2) as superscripts are (1) = x, L"+y, 92'z; (2) = \+x, -y, -zi G) = L.+7,1a-y, \+2. *shared edge between polyhedra. KEEGAN ET AL.: SENEGALITE 1245 Table 4. Senegalite. Anisotropic-thermal vibration parameters parallel to (010). The tetrahedra further link to (x 10,)f chains related by the b-axial glide to form an open polyhedral framework (1976) At on Bzz structure. Johan re- ports an imperfect (010) cleavage.Each tetrahedron Ar(1) 2.4 (r) 1.16(s) 2.8(1) 0.r (r) -0.3(r) (2) 0.0(1) Ar 2.2(r) 1.3s (6) 2.8(1) 0.1(1) -0 3(1) -0 1(1) is associatpdwith three chains,sharing two of its cor- P 2.24(8) r.1r(s) 2.69(7) 0.r(1) -0 2(8) 0.0(l) nerswithin one chain as seenin Figures I and2. 0t1) 2.r(3) r .7(r) 6.s (3) -0.I (2) -0.8(2) 0.4(2) o(2) 4 0(3) r .7(1) 4.6(2) -0.1(2) -0 8(2) 1.0(2) All hydroxyl groups are the points of linkage 0(3) 3.8(3) 1.
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