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And Napb2(OH) (CO3) See discussions, stats, and author profiles for this publication at: https://www.researchgate.net/publication/236669321 Crystal chemistry of basic lead carbonates. III. Crystal structures of Pb3O2(CO3) and NaPb2(OH)(CO3)(2) Article in Mineralogical Magazine · December 2000 DOI: 10.1180/002646100549896 CITATIONS READS 33 164 2 authors: Sergey V Krivovichev Peter C Burns Saint Petersburg State University University of Notre Dame 667 PUBLICATIONS 8,457 CITATIONS 673 PUBLICATIONS 15,217 CITATIONS SEE PROFILE SEE PROFILE Some of the authors of this publication are also working on these related projects: hybrid uranyl-organic compounds View project uranyl peroxide clusters View project All content following this page was uploaded by Peter C Burns on 12 January 2014. The user has requested enhancement of the downloaded file. Mineralogical Magazine, December 2000, Vol. 64(6), pp. 1077–1087 Crystal chemistry of basiclead carbonates. III.Crystalstructures of Pb 3O2(CO3) and NaPb2(OH)(CO3)2 , S. V. KRIVOVICHEV* { AND P. C. BURNS Department of Civil Engineering and Geological Sciences, 156 Fitzpatrick, University of Notre Dame, Notre Dame IN46556-0767 USA ABSTRACT Thecrystal structure sofsynthetic Pb 3O2(CO3) and NaPb2(OH)(CO3)2,havebeen solved by direct methodsand refined to R =0.062and 0. 024,respectiv ely.Pb 3O2(CO3)isorthorhomb ic, Pnma, a = 22.194(3), b = 9.108(1), c =5.7405(8)A Ê , V =1160.4(3)A Ê 3, Z =8.There are four symmetrica lly distinct Pb2+ cationsin irregular coordinat ionpolyhedra due to the effect of stereoacti ve s2 lone- electronpairs. The structure is based upon double [O 2Pb3]chainsof [O(1)Pb 4]and[O(2)Pb 4] oxocentredtetrahedraandCO 3 groups.The [O 2Pb3]chainsare parallel to the c axis,whereas the CO3 groupsare parallel to the (010) plane. NaPb 2(OH)(CO3)2 ishexagona l, P63mc, a = 5.276(1), c =13.474(4)A Ê , V = 324.8(1) AÊ 3, Z =2andhas been solved by direct methods. There are two symmetricallydistinct Pb 2+ cationsin asymmetric coordinat ionpolyhedra due to the effect of stereoactive s2 lone-electronpairs. The single symmetrical lyunique Na + cationis in trigonal prismaticcoordinat ion.The structure is based on hexagonalsheets of Pbatoms. Within these sheets, Pbatoms are located at vertices of a 3 6 net,such that each Pb atom has six adjacent Pb atoms that are ~5.3 AÊ away.Two sheetsare stacked in a close-packingarrangeme nt,forming layers that containthe (CO 3)groups.The layers are linked by OH groupsthat are linearly coordinat edby two Pb2+ cations. Na+ cationsare located between the layers. The structure is closely related to the structuresof other lead hydroxide carbonate s(leadhillite,macpherso nite,susannite, hydroceru ssite, ‘plumbonacrite ’). KEY WORDS: basiclead carbonates, lone-electron pairs, oxocentred tetrahedra, hexagonal lead sublattice Introduction (Roberts et al., 1995). Pb3O2(CO3)isalso known asan intermediateproduct of thermaldecomposi- Thephase PbCO 3 2PbO, or Pb3O2(CO3), was tionof cerussiteto leadoxide (Warne and Bayliss, identied by Roberts et al.(1995)in cerussite- 1962;Grisafe and White, 1964) . bearingmineral specimens from the Grand Reef Thesynthetic phase NaPb 2(OH)(CO3)2 was mine,Graham County, Arizona, USA, inassocia- rstreported by Bulakhova et al. (1972) as a tionwith shannonite and litharge. Although the productofreactionofhydrocerussite, phasehas a naturalorigin, its approval as a new Pb2(OH)2(CO3),with a 2:1mixture of Na 2CO3 mineralspecies awaits discovery of pure material and NaHCO3.Later,Brooker et al. (1983) reportedX -raypowder diffraction data, infrared andRaman spectra for this compound. On the basisof theirdata, Brooker et al.(1983)suggested *E-mail: [email protected] .ru thatthe carbonate groups in NaPb 2(OH)(CO3)2 *Permanent address: Department of Crystallography, arein two non- equivalentsites, and that the St. Petersburg State University, University Emb. 7/9. structurecontains a well-dened hexagonal Pb 199034 St. Petersburg Russia sublattice. # 2000The Mineralogical Society S.V.KRIVOVICHEVAND P.C.BURNS Asa partof our ongoing study of the crystal Two suitablecrystals of the compounds were chemistryof basic Pb carbonates (Krivovichev mountedon a Brukerthree-circle CCD- based andBurns, 2000 a,b),we have determined the X-raydiffractome teroperated at 50 kV and structuresofsyntheticPb 3O 2(CO 3 ) and 40mA. Morethan a hemisphereof three- NaPb2(OH)(CO3)2,andreport the results herein. dimensionaldata was collected using monochro- matic Mo-Ka X-radiationfor each crystal, with framewidths of 0. 3 8 in o,andwith 10 s spent Experimental countingfor each frame. The unit-cell parameters Singlecrystals of synthetic Pb 3O2(CO3) were (Table1) were re ned using least- squarestech- obtainedusingthe procedu redescrib edby niqueswith 1572 and 1510 re ections for Krivovichevand Burns (2000 a).Thecrystals Pb3O2(CO3) and NaPb2(OH)(CO3)2,respectively. occuras colourless needles up to 2. 0mm in Theintensity data were reduced and corrected for lengthand 0.03 mm across. Lorentz,polarization, and background effects Singlecrystals of synthetic NaPb 2(OH)(CO3)2 usingthe Bruker program SAINT. Asemi- wereobtained by hydrothermal methods from a empiricalabsorption-correcti onfor Pb 3O2(CO3) mixtureof 0. 05g ofPbO, 0.05g ofPbCl 2, and wasperformed based upon 696 intense re ec- 0.05g ofPbCO 3 with5 mlof ultrapureH 2O. The tions.The crystal was modelled as an ellipsoid, pHof the solution was adjusted using aqueous whichlowered the Razimuthal from23.1 to 10. 7 %. NaOH to~10. The reactants were placed in a Asemi-empiricala bsorption-correctionfor Teon-lined Parr bomb and were heated to 230 8C NaPb2(OH)(CO3)2 wasperformed on the basis for~24 h. The products were lteredand washed of1340 intense re ections. The crystal was withultrapure water. Several single crystals of modelledas a (001)plate; re ections with a NaPb2(OH)(CO3)2 wereobtained. The crystals plate-glancingangle of <3 8 werediscarded from occuras colourlesshexagonal plates up to 0.7mm thedata set, which lowered the Razimuthal from indiameter and 0.05 mm thick. 27.4 to 4.8%. TABLE 1.Crystallographic data for Pb 3O2(CO3) and NaPb2(OH)(CO3)2. Parameter Pb3O2(CO3) NaPb2(OH)(CO3)2 a (AÊ ) 22.194(3) 5.276(1) b (AÊ ) 9.108(1) c (AÊ ) 5.7405(8) 13.474(4) V (AÊ 3) 1160.4(3) 324.8(1) Space group Pnma P63mc F000 2336 486 m (cm 1) 867.78 518.24 3 Dcalc (g/cm ) 8.17 5.86 Crystal size (mm) 0.2060.0360.04 0.5860.2460.04 Radiation Mo-Ka Mo-Ka Total Ref. 6601 1605 Unique Ref. 1472 342 Unique |Fo| = 4sF 1047 331 R 0.062 0.024 wR 0.170* 0.059** S 1.058 1.058 2 Ý Note: R = S(|Fo| |Fc|)/S|Fo|; S = [Sw(|Fo| |Fc|) /(m n)] , for m observations and n parameters 2 2 2 2 2 * w = 1/[s (Fo) + (0.0987P) ] where P = (Fo + 2Fc)/3 2 2 2 2 2 ** w = 1/[s (Fo) + (0.1170P) + 3.6042P] where P = (Fo + 2Fc)/3 1078 CRYSTAL STRUCTURE OFP B3O2(CO3) AND NAPB2(OH)(CO3)2 Structuresolution and refinement Results Cationcoordina tion TheBruker SHELXTL Version5 systemof Pb3 O2 (CO3) programswas used for the determination and renement of the crystal structures. The structures Thereare four symmetrically independent Pb 2+ weresolved by direct methods and were success - cationsin the structure of Pb 3O2(CO3) (Fig. 1). fullyre ned on the basis of F2 forall unique data in ThePb(1) and Pb(3) cations are coordinated by thespace groups Pnma and P63mc for Pb3O2(CO3) sixO atoms,whereas the Pb(2) and Pb(4) cations and NaPb2(OH)(CO3)2,respectively.The choice of arecoordinated by four and seven O atoms, space group P63mc for NaPb2(OH)(CO3)2 is in a respectively.The coordinati onpolyhedra are goodagreement with the results of spectroscopic stronglydistorted due to the effect of s2 lone studiesby Brooker et al.(1983).The nal electronpairs on the Pb 2+ cations.In both Pb renement converged to an agreement index ( R1) coordinationpolyhedra the location of the lone of0. 062for Pb 3O2(CO3),calculated for 1047 electronpair is apparent from the asymmetry of uniqueobserved ( |Fo|5 4sF)reections, and to thepolyhedra (Fig. 1) .Thetwo symmetrically anagreementindex( R 1)of0.024for independentcarbonate triangles show typical NaPb2(OH)(CO3)2,calculatedfor 331 unique bond-lengths,with a <C O>of1. 30and 1.31 A Ê observed (|Fo|5 4sF)reections. The nal for C(1)O3 and C(2)O3,respectively. atomiccoordinates and anisotropic displacement parametersare given in Tables 2 and3, selected NaPb2 (OH)(CO3)2 interatomicdistances are in Tables 4 and5. The Thereare two symmetrically independent Pb 2+ calculatedand observed structure factors have been cationsin thestructure of NaPb 2(OH)(CO3)2. The depositedwiththePrincipalEditorof geometriesof both coordination polyhedra are MineralogicalMagazine andare available upon similar(Fig. 1) .ThePb(1) and Pb(2) cations are request. eachcoordinated by one OH groupand six O 4 2 TABLE 2.Atomic coordinates and displacement parameters ( 610 AÊ ) for Pb3O2(CO3). Atom x y z Ueq Pb(1) 0.42738(5) 1/4 0.7828(2) 82(4) Pb(2) 0.18557(5) 1/4 0.7855(2) 96(4) Pb(3) 0.32522(4) 0.0487(1) 0.7845(2) 132(3) Pb(4) 0.06986(4) 0.0226(1) 0.7821(2) 140(3) C(1) 0.036(2) 1/4 0.741(6) 120(70) C(2) 0.207(2) 1/4 0.799(6) 180(80) O(1) 0.1279(6) 0.097(2) 0.532(3) 80(30) O(2) 0.1288(5) 0.098(2) 0.034(2) 60(30) O(3) 0.146(1) 1/4 0.785(4) 150(50) O(4) 0.023(1) 1/4 0.787(4) 120(50) O(5) 0.0612(8) 0.125(2) 0.710(3) 220(40) O(6) 0.236(1) 0.127(3) 0.786(4) 410(60) Atom U11 U22 U33 U23 U13 U12 Pb(1) 59(6) 89(6) 97(7) 0 10(4) 0 Pb(2) 47(5) 122(7) 120(7) 0 14(4) 0 Pb(3) 188(5) 83(5) 124(6) 1(3) 7(4) 77(4) Pb(4) 168(5) 150(5) 103(6) 4(3) 10(3) 99(4) 1079 2 TABLE 3.
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