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A NOVEL FACE-SHARING OCTAHEDRAL TRIMER in the CRYSTAL STRUCTURE of SEAMANITE Paur B

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A NOVEL FACE-SHARING OCTAHEDRAL TRIMER in the CRYSTAL STRUCTURE of SEAMANITE Paur B THE AMERIC.\N MINERALOGIST. VOL. 56. SI]PTI'MBER_OCTOBER, 1971 A NOVEL FACE-SHARING OCTAHEDRAL TRIMER IN THE CRYSTAL STRUCTURE OF SEAMANITE Paur B. Moonn, Departmentof the GeophysicalSciences, The Uniaersitlt of Chicago,Chicago, Illi.nois 60637 AND Susnare Guosr, Planetologlt Branch, Goddard Space Fl,ight Center, G'reenbelt,Maryland 2077 1. Assrnacr The atomic arrangementof seamanire,Mnl+(oI{)dB(oH)4][Po{1, a 7.811 (5). 6 15.114(10), r 6 691(5) L, Z:+, spacegroup Pbnm,was deciphered b1. vector set tech- niques.Utilizing 1217independent reflections, full-matrix refinementconverged to Rau :0.062. The structure is basedon a novel face-sharingMn-O octahedraltrimer which links bv edge-sharingwith symmetry equivalent trimers to form infinite chains running parallel to the c-axis Each chain is weakly linked to an equivalent chain through common hy- droxylgroups to form a band.The ligandsinclude (OH)- anions,and tetrahedral[B(OH){l and [POa]groups The tetrahedral groups bridge octahedralbands to form a fairly rigid three-dimensionaledifice. One oxygenatom associatedrvith P doesnot bond to the octa- hedralcations but acceptsfour possiblehydrogen bonds which, with the P5+cation, define a distorted trigonal bipyramid. The peculiartrimer is apparentlystabilized by the shortO-O'edge associated rvith the borate tetrahedron. Of the three trimeric face-sharingoctahedral isomers, two are no$ known to exist in natural crystals ItTrnooucrror.I Seamanite, a rare hydrated borate-phosphate of manganese, was first described by Kraus, Seaman, and Slawson (1930). It occurred in frac- tures cutting siliceous rock at the Chicagon Mine, Iron River, Michigan, as pale pink to yellow acicular crystals associated with sussexite, man- ganic oxyhydroxides, and calcite. Few specimens were preserved, most of which appear in the A. E. Seaman Mineralogical Museum at Michigan Technological University. McConnell and Pondrom (1941), by X-ray study and etch tests, establisheda 7.83 (2), b 15.I4 (2), c 6.71 (2), space group Pbnrn On the basis of powder photographs, they further con- cluded that seamanite, believed to be Mq(BOB) (POD.3H2O, was prob- ably not isostructural with reddingite, Mq(PO4)2'3H2O. As part of a general program concerning octahedral clustering in manganese anisodesmic oxysalts, we report a detailed study of the seamanite atomic arrangement. We wish to remind readers that the rarity of a specieshas little bearing on the significance of formal crystal structure analysis directed toward furthering our knowledge of crvstal chemistry. As a point of fact, some of the most unexpected clusters have t527 ls28 MOORE AND GEOSE been revealed only through the study of more exotic species.Seamanite proved no exception; not only have we found a novel octahedral face- sharing cluster hitherto believed impossible on geometrical grounds, but we are also committed to interpret the seamanite crystal-chemical for- mula as a basic compound with composirion Mry2+(OH)r[B(OH).][POI]. ExprnnmNur- A nearly perfectly symmetrical rectangular prism (U.S. National Museum No. 96282) of 0.005 mmt volume was selected for study. 3000 reflections with c as the rotation axis were collected on a PATLRED automated difiractometer using a graphite monochromator and Mo radiation to 20:650. The cell parameters in Table 1 were obtained from con- ventional least-squares refinement of the indexed powder data in Table 2. These powder data were obtained from a spherical powder mount utilizing a 114.6 mm diameter Buerger camera and Mn-filtered Fe radiation, and the corresponding Miller indices were un- ambiguously selected by comparison with the strong intensities of the single crystal study. Individual single crystal integrated intensities were obtained using a 1.8o half-angle scan, with background counting time on each side of the peak of.20 seconds. Reflection pairs of the kind I (hkl) , I (ilkl) were averaged since o-scans about the basal reflections revealed that absorption anisotropy correction amounted to only 6 percent of the mean peak value. A total of 1217 s)'nmetry independent non-zero reflections were processed and were the only ones used in the ensuing study. Among the remaining 515 zero-reflections were the space group absences as well as weak data which were within the error of the background difierences and these data were excluded from further considera- tion. TABI,E 1. SEAIANITE: CRYSTAI, CELL DATA ed) 7.8rr (s) !. (8) Is.1r4 (10) s. (8) 6.6er (s) v 63) 7e0.0 (7) 6pace group B!lg, . tr 1 fomula le'3(olD z [B(o]D nl LnouJ z 4 specific gravityl 3.128 calc 3.L32 gry'cn3 I -Kraus,I Seaman and SLawson (1930). STRUCTURE OF SEAMANITE TABLE 2. SEAI'AMTE: PO{DER DATAa r_/r_o d(obs) d (calc) lEl 6 7.551 7 .557 020 10 6.917 6:939 ll0 5 5 .420 5 .43r 120 5 4.807 4.817 u1 6 4.204 4.2L7 l2r 5 3.899 3.906 200 3.777 3.781 210 6 3.467 3 .469 220 5 3.394 3 .401 140 3 3.313 3 .345 oo2 3 3.286 3 .290 04r 5 3.057 3.059 o22 8 2.843 2.848 L22 2 2.7L3 2.7L5 240 3 2.6L7 2.625 132 ? 2.58r 2.566 3r0 2 2.555 2.5r9 060 2.502 2.506 2L2 6 2.393 2.397 160 I 2 .3sl 2.357 06I 2 2.309 2.310 32L 3 2.263 2.269 232 2 2.184 2 .186 331 4 2.III 2.LI7 260 2.108 242 I 2.073 2.08I L70 2 2.061 2.063 L23 I 2.O25 2.036 3L2 2 2.0r5 2.018 26I 2.OL? 062 I L.974 I.987 t7r I r.9 45 1.945 252 5 1.901 1.903 332 I I.818 1.8I8 27L 2 1.769 L.77L 181 1530 MOORL:,AND GHOSIi TABLE 2. (contintled)' T,/T g (cale) --o $(obs) ILl I t_.736 L.735 440 t I.687 1.687 402 l+ L.672 r.6 76 4L2 r.673 004 r.643 I.645 082 a r.6 36 1.640 450 3 1.610 1 .6r0 182 1.594 1.592 362 z r.5r+2 1.543 290 3 r.528 r.529 380 I.529 520 I I.502 1.501 144 1.488 r.488 372 I I.4I9 I.4I8 183 z 1.402 1.401 311+ 1.401 292 L"372 I.372 164 I .371 254 r.330 r.329 472 1.325 L.326 542 L.322 193 I 1"304 1.302 600 2 L"262 1 .260 630 l_ r .25r+ L.252 084 t F"K* ; 114.6 mrncamera dianeter. Filrn conrected fon shrinkage. When morb than one reflection contributes to d(obs), all are listed in decreasing value of spacing. ST'RUCTURE OF SI.:.A M A N IT li 1531 Sor,urron ol tun Srnucrunp Patterson projections, P(ua) and P(z'ru), combined with polyhedral packing models assisted in the structure determination. The only hindrance in the experiment was the prejudice on the part of the investigators that the clusters revealed by vector set analysis were crystallochemically impossible and were rejected in the initial trial parameter refine- ments, thus rendering the problem more costly in time than justified. The correct model, consisting of two s)zmmetry independent Mn atoms and one P atom, yielded a heavy atorn least-squares refinement of Iiir*,"1- Roo,: _ =:2 la","ll:0.28 p_ Difierence synthesis of the phases thus produced unambiguousiy revealed all oxygen atoms in the asymmetric unit of the crystal structure. Inclusion of the anions in the refinement followed by further difference synthesis revealed the position of the boron atom. RerrntlmN:r The study by McConnell and Pondrom (1941) indicated a centrosynmetric crystal and we did not find it necessary to consider lower s],'rnmetry throughout this study. AII atomic free parameters in the asymmetric unit were refined according to full-matrix least-squares procedures using a local version of the familiar program of Busing, Martin, and Levy (1962). Scattering curves for Mnl+, P3+, B2+, and Or- r,r'ereobtained from MacGillavry and Rieck (1962). The reliability index, R7,47,converged to 0.O62 Ior alI 1277 non-zero reflections which were each ascribed unit weight. The atomic coordinates and isotropic -f'",r" thermal vibration parameters are listed in Table 3 and the lF.o"l data appear in Table 4.1A ratio of independent data to variable parameters of 30:1, Iow estimated stan- dard errors for the atomic parameters and thermal vibration parameters typical for their ionic speciesadd confidence to the interatomic distances discussed further on. DnscnrprroN oF THE Srnucrune Seamanite is certainly a candidate for one of the most exotic of min- eral structures. The Mn-O octahedral arrangement is one of the most peculiar and unexpectedon record,and we shall discussit in detail. Figure 1 features a polyhedral diagram of the octahedral backbone and its surrounding tetrahedral [B(OH)4] and [PO4]ligands, projected down the ,r-axis.We isolate the octahedral backbone and show it in Figure 2. It consistsof an octahedralface-sharing trimer which jcins to identical trimers by reflection across shared edges.The resulting chain runs parallel to the prismatic c-axis of the crystal. The face-sharing trimer is the most peculiarfeature of the structure sinceits arrangement on geometrical grounds utilizing regular octahedra with oxygen atoms I To obtain a copy of Table 4, order NAPS Documdnt 101519from National Auxiliary Publications Service of the A.S.I.S., c/o CCM Information Corporation, 909 Third Avenue, New York, New York 10022; remitting $2.00 for microfiche or $5.00 for photo- copiespayable to CCMIC-NAPS.
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