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The Crystal Structure of Faustite and Its Copper Analogue Turquoise

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The Crystal Structure of Faustite and Its Copper Analogue Turquoise Mineralogical Magazine, October 2000, Vol. 64(5), pp. 905–913 The crystal structure of faustite and its copper analogue turquoise U. KOLITSCH* AND G. GIESTER Institut fu¨r Mineralogie undKristallographie, Geozentrum, Universita¨t Wien, Althanstr. 14, A-1090 Wien, Austria ABSTRACT The crystal structure of faustite, ZnAl6(PO4)4(OH)8Á4H2O, was determined using single-crystal data (Mo-Ka X-radiation, CCD area detector, 1624 unique reflections, R1 = 4.91%, wR2 = 9.23%), and comparedwith results of a reinvestigation of the structure of its copper analogue turquoise, CuAl6(PO4)4(OH)8Á4H2O (2737 unique reflections, R1 = 2.81%, wR2 = 6.90%). Both are isostructural andcrystallize in space group P1¯, with a = 7.419(2) [turquoise: 7.410(1)], b = 7.629(3) [7.633(1)], c = 9.905(3) [9.904(1)] A˚ , a = 69.17(2) [68.42(1)], b = 69.88(2) [69.65(1)], g = 64.98(2) [65.05(1)]8, V = ˚ 3 462.2(3) [460.27(10)] A , and Z = 1. The structure consists of distorted MO6 polyhedra (M = Zn, Cu), AlO6 octahedra and PO4 tetrahedra. By edge- and corner-sharing of these polyhedra a fairly dense three-dimensional framework is formed which is further strengthened by a system of hydrogen bonds. The metal atoms in the unique MO6 (M = Zn or Cu) polyhedron show a distorted [2+2+2]-coordination, the distortion being more pronounced in turquoise. About 10% of the M site is vacant in both minerals. In turquoise, a previously undetected structural site with a very low occupancy of (possibly) Cu is present at the position (Ý,0,Ý). KEYWORDS: faustite, turquoise, crystal structure, crystal chemistry, phosphates. Introduction from the Iron Monarch iron ore deposit in South Australia (Pring et al., 2000). The pale brownish FAUSTITE, ZnAl6(PO4)4(OH)8Á4H2O (Erd et al., rose to colourless, platy or prismatic faustite 1953), is the rare Zn analogue of turquoise, crystals (up to 0.1 mm) are accompaniedby CuAl6(PO4)4(OH)8Á4H2O, with which it forms a hausmannite andkleemanite, solidsolution series. Both belong to the turquoise ZnAl2(PO4)2(OH)2Á3H2O. Chemical analyses group which also includes the members chalco- have demonstrated (Pring et al., 2000) that the 3+ siderite, CuFe6 (PO4)4(OH)8Á4H2O, aheylite, faustite contains little or no copper andonly very 2+ 3+ (Fe ,Zn)Al6(PO4)4(OH)8Á4H2O andplanerite, small quantities of iron (probably Fe substi- &Al6(PO4)2(PO3OH)2(OH)8Á4H2O(& = tuting for Al; see FoordandTaggart, 1998). The vacancy) (see recent review of Foordand present article reports the refinement of the crystal Taggart, 1998 for further details). The crystal structure of one of these faustite crystals. For structure of faustite has not been verifiedor comparison purposes, we also reinvestigatedthe refinedto date,although it was assumedto be crystal structure of turquoise because the earlier isostructural with turquoise, which hadbeen structure determination (Cid-Dresdner, 1965) determined to be triclinic, with space group P1¯ reportedunusually large ranges for the Al ÀO (Cid-Dresdner, 1965; R = 7%). andP ÀO bondlengths. Recently, the first occurrence of single, well- developed crystals of faustite has been reported Experimental A very small chip cut from a colourless single crystal of faustite was selectedfor the structure * E-mail: [email protected] analysis. The crystal chip with the approximate # 2000 The Mineralogical Society U. KOLITSCH AND G. GIESTER dimensions 0.1060.0560.03 mm was mounted A pale bluish crystal of turquoise with the on a Nonius KappaCCD diffractometer equipped approximate dimensions 0.1260.0860.05 mm with a 300 mm diameter capillary-optics colli- was chosen for the reinvestigation of the turquoise mator for improvedresolution. Preliminary structure. The crystal was taken from a specimen investigations gave a triclinic unit cell very showing well-developed, pseudorhombohedral similar to that reportedfor turquoise (Cid- crystals, also from Iron Monarch, South Dresdner, 1965). For the intensity data collection Australia. Semiquantitative energy-dispersive at room temperature, we employedMo- Ka chemical analyses of three different turquoise X-radiation (l = 0.71073 A˚ ) anda detector crystals showedthem to contain only traces of Zn, distance of 28 mm. Using j and o as rotation K or Ca as impurity elements. The selected axes (rotation width 28), 382 data frames were turquoise crystal was measuredundervery similar aquired, each collected over 365 s (see Table 1 conditions (see above and Table 1). A triclinic for further details). The data were processed using unit cell was foundwhich was very similar to that the Nonius program suite DENZO-SMN and reportedby Cid-Dresdner(1965). Again, no correctedfor Lorentz, polarization andback- absorption correction was applied. Normalized groundeffects. Because of the small absorption structure factor statistics indicated the centrosym- coefficient, m = 2.12 mmÀ1, andthe small size of metric space group P1¯ for both faustite and the crystal chip used, no absorption correction turquoise crystals, in agreement with the observed was applied. crystal habits. TABLE 1. Crystal data, data collection information, and refinement details for faustite and turquoise. Faustite Turquoise Formula (simplified) ZnAl6(PO4)4(OH)8Á4H2O CuAl6(PO4)4(OH)8Á4H2O Formula weight 815.26 813.43 Space group P1¯ P1¯ a, b, c (A˚ ) 7.419(2), 7.629(3), 9.905(3) 7.410(1), 7.633(1), 9.904(1) a, b, g (8) 69.17(2), 69.88(2), 64.98(2) 68.42(1), 69.65(1), 65.05(1) V (A˚ 3), Z 462.2(3), 1 460.27(10), 1 F(000) 408.0 407.0 m (mmÀ1) 2.12 1.98 À3 rcalc (gÁcm ) 2.929 2.935 Data collection andrefinement Total no. of frames 382 304 Collect. time per frame (s) 365 220 Collection mode sphere sphere ymax (8) 30.0 (used: 25.03) 30.49 h, k, l ranges À8 ? 8, À9 ? 9, À11 ? 11 À10 ? 10, À10 ? 10, À13 ? 13 Total refls. measured4389 5193 Unique reflections 1624 2737 R1(F), wR2(F2) 4.91%, 9.23%* 2.81%, 6.90%{ ‘Observed’ refls. 1443 [Fo >4s(Fo)] 2437 [Fo >4s(Fo)] Extinct. factor - 0.0173(16) No. of refinedparameters 211 213 ‘Goodness of Fit’ (GoF) 1.212 1.106 (D/s)max 0.0001 0.0001 ˚ 3 Drmin, Drmax (e/A ) À0.49, 0.52 À0.60, 0.75 Note: Unit-cell parameters were refinedfrom all recordedreflections.Scattering factors for neutral atoms were employedin the refinement. 2 2 2 2 2 * w = 1/[s (Fo ) + (0.02P) + 1.9P]; P = ([max of (0 or Fo )] + 2Fc )/3 { 2 2 2 2 2 w = 1/[s (Fo ) + (0.02P) + 0.5P]; P = ([max of (0 or Fo )] + 2Fc )/3 906 CRYSTAL STRUCTURE OF FAUSTITE The positions of the metal andoxygen atoms in The final refinement cycle for faustite ledto R1= faustite were locatedusing directmethods 4.91%, wR2 = 9.23%. Final R factors for (SHELXS-97, Sheldrick, 1997a) andsubsequent turquoise were R1 = 2.81%, wR2 = 6.90%. Fourier anddifferenceFourier syntheses. The Residual electron densities in both crystals were deduced structure model is basically that of <+1 e/A˚ 3. The final positional anddisplacement turquoise (Cid-Dresdner, 1965). Further differ- parameters are presentedin Tables 2 and3, and ence Fourier syntheses revealedall 8 H atoms selectedbondlengths andangles in Table 4. present in the unit cell. The positions of the H Probable hydrogen bonds are listed in Table 5. atoms given here are those which are in fact Results of empirical bond-valence calculations bonded to the respective O atoms, and not the (Brown andAltermatt, 1985; Brese andO’Keeffe, symmetry-equivalent positions as listedin Cid- 1991; Brown, 1996) are given in Table 6. Lists of Dresdner (1965). Full-matrix least-squares refine- observedandcalculatedstructure factors ment on F2 (SHELXL-97, Sheldrick, 1997b), (Table 7) have been deposited with the Editor. involving anisotropic displacement parameters for all non-H atoms, gave a discrepancy factor R1of ~6%. At this stage, residuals of the electron Discussion density were in the range of +1 e/A˚ 3. The Structure connectivity and cation coordinations refinement of turquoise proceeded in the same The structure contains distorted MO6 polyhedra way, with R1 & 3.5% in the later stages of the (M = Zn, Cu), AlO6 octahedra and PO4 tetrahedra. refinement andelectron density residuals The dominant structure element is an ˚ 3 <+1.2 e/A . [Al2MAl2(O,OH,H2O)18] polyhedral cluster The approximate Zn:Cu ratio in the faustite formedby a central MO6 polyhedron sharing crystal chip measuredwas then determinedafter four edges with two edge-sharing Al(1)O6- the data collection by semiquantitative energy- Al(2)O6 dimers (Fig. 1). The AlO6 octahedra in dispersive X-ray analysis, giving a value of ~10:1. the cluster are corner-linkedto the Al(3)O 6 Additional point analyses of one small cluster of octahedron which shares Oh(9) with Al(1)O6 faustite crystals showedthat the Zn:Cu ratio can and MO6, andOh(12) with Al(2)O 6 and MO6. be fairly variable (probably even within a single Further corner-linkage via the two non-equivalent crystal), ranging from ~12:1 to ~3:1. Very minor Fe was detected in both the measured crystal and the crystal cluster. It is known that both turquoise andfaustite form a complete solidsolution series with planerite, &Al6(PO4)2(PO3OH)2(OH)8Á4H2O (i.e. a member of the turquoise group with dominant vacancies on the transition metal site), andthat cuprian planerite is in fact more common than turquoise (FoordandTaggart, 1988). Accordingly, we refined the occupancy of the M (M = Zn, Cu) site in faustite andturquoise, neglecting the very minor Cu-for-Zn substitution in faustite. The occupancy factors obtainedwere 0.927(5) and0.874(2) for faustite andturquoise, respectively, indicating that the M site contains 7 and13% vacancies.
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