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Crystal Structure of Ca2na2(CO3)3 (Shortite)

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Crystal Structure of Ca2na2(CO3)3 (Shortite) JOURNAL OF RESEAR CH of th e Notional Bureau of Standards-A. Physics and Chemistry Vol. 75A, No. 2, Marc h ~ Ap ril 1971 Crystal Structure of Ca 2 Na 2 (C03 )3 (Shortite) B. Dickens, A. Hyman, * and W. E. Brown** Institute for Materials Research, National Bureau of Standards, Washington, D.C. 20234 (December 18, 1970) Ca, N",(CO"h cryS la lli ze, in I he o rl hnrhombic un il ce ll (f = 4.947( I ) A. /) = I 1.0:)2(2) A. a nd (" = 7. 108( 1) A al 2S oC wi lh 111'1) formul a weip:ll is in s l' aee·p:rtlup Am 1ll 2. Th" , Irue lu re has been J"( ·delcrm in ed. ("o ITeel,·d. a nd rdined 10 /? ".= 0.02S . /? = 0.020 u s in ~ 684 "ol,,;erved" x· ray reflec li ons f rom a s ill ~. .d(' ('ry!-' I al. Corrcctions w('r(' m uck ror a bsorption a nd isol rllpic t'xlinclioll . III the t'xtinc tio n refin e me nl s, ,. refin e d 10 0.000]7(1) C Ill. The structure consists of Ca,NaCO" layers inte rl eaved with Na(CO,,), laye rs . T he Ca ion is coordin a led sl r o n ~ l y 10 nin e oxygcns, in c ludi,;g Ihree LO" edges, wilh Ca .. 0 di s lalHTs varyin g from 2.40 1(2) ;\ In 2.S76(2) A. One Na io n is cuurd in a lcd sl ronp:ly 10 e ighl oxyp:cns , In c lud ing 111'0 CO" e dges. wilh Na ... ° rii sla n.ops from 2.429(2) A1 02.605(1) A. The 01h e r Na io n i, coordi nal(' c1 slrun;;!y In six ox y~ en , . incilidi np: one CO" edp:e . a l 2.296( 1) A 10 2.414 A. a nd wea kly 10 a sevenlh a l 3.050(3) A. One CO" P: r<lUI' is coordinaledlo seve n cal ions . Ihe ol hc r is coordin a led 10 ( ' i ~ hl. Tht' CO:1 g r n up ~ havl' s l'(, Jllill ~ l y max imi zed the ir ('dge =-- haring with Ca inns ratla'r tha n Na io ns. ~ ('y words : Calci um ~o dilllll ca rbonat(': cr ys tal :-; trtl C' tul"(': shortit e: sin :,r k -(' r ysl al x-ray diffracti on, 1. Introduction fr agment from mine ral sa mple 105807, National Museum of Natural Hi sto ry, Smithsoni an InstituLion, As part of a progra m of s tudies [1 , 2J I 10 obtain pre­ Washington , D.C. (sample s uppli ed by J. S. White, Jr. ). cisc Slructura l parame le rs on calcium carbonates, The sphe re was mounted on Ih e go ni o me te r head in ca lcium carbo natc hyd r ates, calciu m phosphal es, a nd ou r usua l way r2]. re laled co mpounds, we have re in vesti gated Ih e crystal formu la (id eal): Ca~ Na~ (C01 h structure of Ca~Na~(CO : lh, whi ch exists in nature as cell: orthorh ombic the min e ral sho rtite. The s truc lura l fealures in these a, = 4.947(1) A compo unds are import ant in the cons id eration of pos­ b = 11.032(2) A sible e pit ax ial, syntaxial, a nd substitu tional solid solu­ c = 7.108(1) A tion. re lali onsh i ps in I he majo r ino rganic phases found vo lume = 387.9 A.:l in VI VO. s pace-grou p A mm2; S ho rlil e was firs t found [3] in a matri x of montmoril­ cell conte nts 2 [ Ca~Na2(C0 3h ] lonite clay whi c h also contai ns pyrite (FeS~), calcit e reciprocal lattice extin ctions : k + l = 2n + l for (CaCO:1) , and a carbonate of magnesium in c rys tals hkL ; which were too s mall to be ide ntifi ed. Massive de posits calculated density 2.620 g' cm-:l; 3 of the commerciall y important mineral trona (Na~C O :l . observed density 2.629 g ' c m- [3]. NaHCO:1 · I-I ~ O ) are also found in the vicinity. A c rystal The procedure given in reference [2] was followed structure for s hortite has been reported by Wickman in the collection a nd processin g of data with the follow­ [4], who s uggested ato mi c positi ons on the basis of ing exceptions. The &--28 scans were carried out at refracti ve indices, spati al considera ti ons, a nd the 2°/ min. Eac h background was counted for 20 s. 1659 intensiti es o f the OkL re fl ections. Wc found this struc­ reflec tio ns we re coll ected from the Ilkl a nd hkL octants ture to contain one in correcl feature. The corrected and were me rged in to a unique set of 711 , of which structure of shorlil e is re ported here. 684 a re "observed" and 27 are " unobserved." The R fa c tur be tw een observed equivalent reAecti ons was 2. Data Collection and Structure Refinement 0.01 . No absorption corrections were made because the maximum e rror in an inte nsity due to absorption The crys ta l used in the data coll ecti on is a n approxi­ is 0.8 pe rcent. For Ca~Na~(CO:lh, f-t (Mo) = 15.7 c m ~ l. male s phere, radius 0.112(4) mm , ground from a s hortite The Picke r ~ hardware dropped the least s ignifi cant "! Certai n cO lllmercial ('quipmt'llt. in s truments . or ·materials a rc ide ntified in this p aper *Dl'part 1!l t.: ll t of CIH'llIi .-.; t r y. Ulliversity of \ \ary\alld Bah illlnrt.' C nllnlY. Bctltimon'. Md. i ~ l or.der to specify the experimental procedure adequately. In no case ri oes s uc h id e nt iftca­ ** Din,(· tol". Arn eril" an Dental As~ol"iatioll H t.:~t'a r (' h Pl"Ogralll. National Bu reau of S tand· tilin Imply recom mendat ion 01" endorsf' me nt b y the Nat ional Bureau of S ta ndards . nor does arcls. Washington. D.C. 20234. it imply that the material or eq uipment ide ntified is necessarily the best available fo r the 1 Fi )! III"e:'!' ill br a(" k( , t ~ indicate t hl' lit. 'I"<l ture rd{"l't'Il(. T ~ a t till' (' nd oft hi ::. pap!'l". pu rpose. 129 413-992 0 - 71 - 3 digit during the data collection so that the standard tween the extinction parameter and the scale factor. deviations from counting statistics, and consequently All other correlation coefficients are less th an 0.28. our assessment of whether a given reAe ction is ob­ The atomic parameters are given in table 1. All served or unobserved, is only marginally correct. This atoms but 0(2) lie in speciaJ positions; the Wyckoff affects very few reAections in the present case because · symbol and symmetry of these positions are given in the sample scattered strongly and nearly all re Aections table 1. The observed and calculated structure factors, were unequivocally "observed" (modified hardware uncorrected for extinction, are given in table 2. was used in later investigations). rr(F) was define d as F/lO for F < 10; 1 for 10 < F < 43; andF/43 for F > 43, 3. Description of the Structure where Fmax was 211; weights in the least-s quares re­ fin ements were 1/rr2 . Wickman's structure [4] for Ca2Na2(C03h would not refi ne to a residual, R w , The structure of CatNa2(C03)3 is shown in figures below 0.3. Examination of the Patterson function and 1 and 2. There are Ca2NaC03 layers at x = 0.5 and an Fo electron density Fourier synthesis phased from Na(CO:;h layers at x = O. The COa group containing structure factor calculations using the positions of C(2), 0(3), 0(4), and 0(4') lies on the mirror at x = 0.5 the Ca and Na ions suggested new positions for the and is a member simultaneously of three cation-anion C(1) and 0(1) atoms. This structure was refined iso­ chains in which cations are coordinated to edges and tropically to Rw = 0.056, R = 0.050, and anisotropically opposite apexes of the C03 group. One CaC03 chain to Rw = 0_030, R = 0.023 and then to R w= 0_025, runs parallel to [011], one runs parallel to [OIl], and R = 0.020 wilh refinement on the isotropic extinction one NaC03 chain runs parallel to [001]. Similar cation­ parameter, r, in additi on to the previously varied anion chains are present in the barytocalcite phase of parameters. The least-squares program RFINE written BaCa(C03 h [8]. The bonding of the apex of the CO:) by Finger [5] was used. Only observed reAections were group in the NaCO:) chain to Na is weak, however. The used in these xefinements. The scattering factors for C03 group containing C(l), 0(1),0(2), and 0(2'), which the neutral atoms were taken from Cromer and Mann is onJhe mirror at x=O and has its plane parallel to (011) [6]. No corrections for anomalous dis persion were or (011), forms N aC03 chains like those cation-anion made_ The fina l value of r is 0.00017(1) c m where chains at x = 0.5.
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