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The Crystal Structure of Zigrasite, Mgzr(PO4)2(H2O)4, a Heteropolyhedral Framework Structure

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Mineralogical Magazine, June 2010, Vol. 74(3), pp. 567–575 The crystal structure of zigrasite, MgZr(PO4)2(H2O)4, a heteropolyhedral framework structure 1, 2 F. C. HAWTHORNE * AND W. B. SIMMONS 1 Department of Geological Sciences, University of Manitoba, Winnipeg, Manitoba R3T 2N2, Canada 2 Department of Earth and Environmental Sciences, University of New Orleans, New Orleans, Louisiana 70148, USA [Received 28 April 2010; Accepted 1 July 2010] ABSTRACT ˚ The crystal structure of zigrasite, ideally MgZr(PO4)2(H2O)4, a 5.3049(2), b 9.3372(4), c 9.6282(5) A, ˚ 3 À3 a 97.348(1)º, b 91.534(1)º, g 90.512(4)º, V 472.79(5) A , Z = 2, triclinic, P1, Dcalc. 2.66 g.cm , from the giant 1972 pocket at Newry, Oxford County, Maine, USA, has been solved and refined to R1 3.75% on the basis of 2623 unique reflections (Fo >4sF). There are two P sites, each of which is solely occupied by P with <PÀO> distances of 1.532 and 1.533 A˚ , respectively. There are two Mg sites, both of which are occupied by Mgand are octahedrally coordinated two O anions and four (H 2O) groups with <MgÀO> distances of 2.064 and 2.075 A˚ , respectively. There is one Zr site, occupied by Zr and ˚ octahedrally coordinated by six O anions with a <ZrÀO> distance of 2.065 A. The (ZrO6) octahedron shares corners with six (PO4) tetrahedra, forminga [Zr(PO4) 2] sheet parallel to (001). These sheets are stacked in the c direction and linked by (MgO2(H2O)4) octahedra that share O atoms with the (PO4) groups. The structure is formally a heteropolyhedral framework structure, but the linkage is weaker in the c direction, accountingfor the marked (001) cleavage. KEYWORDS: zigrasite, phosphate, crystal structure, Newry pegmatite, Maine, malhmoodite Introduction Experimental details ZIGRASITE, MgZr(PO4)2(H2O)4, was described as a The single crystal of zigrasite used in this work, a new mineral from the giant 1972 gem tourmaline- pale tan fragment with dimensions bearingpocket at the Dunton Quarry, Newry, 25 mm660 mm6100 mm, was removed from a Oxford County, Maine, USA, by Hawthorne et al. polished thin section. Electron microprobe analysis (2009). It occurs as complex aggregates of three subsequent to collection of the X-ray intensity data distinct phases, zigrasite and two unnamed showed it to be uniform and close to end-member phases: the Ca analogue of zigrasite, CaZr(PO4)2 composition. The crystal used for structure (H2O)4, and Zr(PO3OH)2(H2O)4. Zigrasite is determination was analysed, usinga Cameca SX- associated with tourmaline, microcline, quartz, 100 electron-microprobe, by Hawthorne et al. albite, beryl, amblygonite-montebrasite, chil- (2009). Determination of the crystal structure (see drenite-eosphorite and apatite, and crystallized below) shows that zigrasite contains four (H2O) as one of the last minerals duringpocket groups per formula unit, and the empirical formula formation. for zigrasite was calculated on the basis of 12 anions including4 (H 2O) groups per formula unit: 2+ (Mg0.97Fe0.01Zn0.01)S=0.99(Zr0.99Hf0.01)S=1.00 P2.00O8(H2O)4,ideallyMgZr(PO4)2(H2O)4. * E-mail: [email protected] DOI: 10.1180/minmag.2010.074.3.567 # 2010 The Mineralogical Society F. C. HAWTHORNE AND W. B. SIMMONS Data collection and crystal-structure ref|nement four O anions with <PÀO> distances of 1.532 and 1.533 A˚ , respectively, close to the grand <PÀO> The single crystal of zigrasite was mounted on a distance in minerals of 1.537 A˚ given by Bruker AXS SMART APEX diffractometer Huminicki and Hawthorne (2002). There are equipped with a CCD detector and usingMo- Ka two Mg sites, both of which are occupied solely radiation. The intensities of 5497 reflections were by Mgand are octahedrally coordinated by two O collected to 60º2y using30 s per 0.2º frame, and an anions and four (H2O) groups with <MgÀO> empirical absorption correction (SADABS, distances of 2.064 and 2.075 A˚ , respectively. Sheldrick, 1998) was applied. The refined unit- There is one Zr site, solely occupied by Zr and cell parameters for the triclinic cell (Table 1) were octahedrally coordinated by six O anions with a obtained from 6768 reflections with I >10s.The <ZrÀO> distance of 2.065 A˚ . crystal structure of zigrasite was solved by direct There are 12 anion sites in the structure of methods with the Bruker SHELXTL Version 5.1 zigrasite (Table 2), labelled O(1) to O(12). The system of programs (Sheldrick, 1997) and refined incident bond-valence sums from the P, Mgand in space group P1¯ to R1 = 3.65% and a GooF of Zr cations in the structure to these anions fall into 1.018. Refinement of the structure was based on two groups: O(1) to O(8) lie between 1.64 and 2623 intensities of unique observed reflections (Fo 2.00 v.u. (valence units) and O(9) to O(12) lie >4sF). Scatteringcurves for neutral atoms were between 0.30 and 0.42 v.u. (Table 4). taken from the International Tables for X-ray Accordingly, O(1)ÀO(8) are assigned as O Crystallography (1992). R indices are given in anions and O(9)ÀO(12) are assigned as (H2O) Table 1, and are expressed as percentages. Details groups. In accord with this assignment, eight H of the data collection and structure refinement are atoms were located at the final stages of structure given in Table 1, final atom parameters are given in refinement and their parameters were refined with Table 2, selected interatomic distances and angles the soft constraint that the O(donor)ÀH distance in Table 3, and bond-valence values in Table 4. A be close to 0.98 A˚ . The stereochemistry of the list of observed and calculated structure factors has resulting hydrogen-bond arrangement is given in been deposited with the Principal Editor of Table 3. Mineralogical Magazine and is available from www.minersoc.org/pages/e_journals/dep_mat.html. Structure topology The Zr octahedron shares corners with six (PO4) Description of the structure tetrahedra to form a pinwheel cluster (Moore Atom coordination 1973) that we may express in its most general [6] [4] There are two P sites, each of which is solely form as [ M( TO4)6]. In zigrasite, this cluster occupied by P and tetrahedrally coordinated by forms a fragment of a [Zr(PO4)2] sheet (Fig. 1) TABLE 1. Miscellaneous information for zigrasite. a (A˚ ) 5.3049(2) Crystal size (mm) 25606100 b 9.3372(4) Radiation/monochromator Mo-Ka / graphite C 9.6282(4) No. of reflections 14396 a (º) 97.348(1) No. in Ewald sphere 5497 b 91.534(1) No. unique reflections 2766 g 90.512(1) No. Fo >5s(F) 2623 ˚ 3 V (A ) 472.79(5) Rmerge % 1.6 Space group P1¯ R1 % 3.75 Z 2 wR2 % 8.72 3 Dcalc (g/cm ) 2.66 Cell content 2 [Zr(PO4)2Mg(H2O)4] R1 = S(Fo À Fc)/SFo 2 2 Ý wR2 =[SwFo À Fc) / Sw Fo ] , w =1 568 2 TABLE 2. Atom positions and displacement paramters (A˚ ) for zigrasite. xyzUeq U11 U22 U33 U23 U13 U12 Zr 0.25362(4) 0.74773(3) 0.49040(2) 0.00794(9) 0.00537(13) 0.00899(13) 0.00943(13) 0.00079(8) À0.00038(8) À0.00084(8) P(1) 0.26500(14) 0.45008(8) 0.68108(8) 0.0129(2) 0.0104(3) 0.0144(3) 0.0137(3) 0.0016(3) À0.0005(3) À0.0010(3) P(2) 0.23232(14) 0.06111(8) 0.32252(8) 0.0123(2) 0.0102(3) 0.0132(3) 0.0133(3) 0.0014(3) À0.0003(2) À0.0013(3) THE CRYSTAL STRUCTURE OF ZIGRASITE Mg(1) 0 0 0 0.0185(3) 0.0126(7) 0.0290(8) 0.0139(7) 0.0030(6) À0.0010(5) À0.0030(6) Mg(2) Ý Ý 0 0.0199(3) 0.0179(7) 0.0242(8) 0.0168(7) 0.0004(6) À0.0017(6) À0.0002(6) O(1) 0.3139(5) 0.5903(3) 0.6181(3) 0.0234(5) 0.0225(12) 0.0209(11) 0.0280(12) 0.0073(9) 0.0006(9) À0.0004(9) O(2) 0.2402(4) 0.4846(3) 0.8389(2) 0.0197(5) 0.0173(11) 0.0272(12) 0.0140(10) 0.0010(8) À0.0005(8) 0.0020(9) O(3) 0.4845(4) 0.3458(3) 0.6475(2) 0.0195(5) 0.0165(11) 0.0217(11) 0.0205(11) 0.0026(9) 0.0025(8) 0.0055(9) O(4) 0.0220(4) 0.3765(3) 0.6176(3) 0.0228(5) 0.0159(11) 0.0254(12) 0.0254(11) À0.0014(9) À0.0035(9) À0.0062(9) O(5) 0.0048(4) 0.1546(3) 0.3686(3) 0.0219(5) 0.0169(11) 0.0233(12) 0.0248(11) À0.0003(9) 0.0040(9) 0.0035(9) O(6) 0.2539(4) 0.0557(3) 0.1641(2) 0.0188(4) 0.0136(10) 0.0286(12) 0.0145(10) 0.0043(8) 0.0009(8) 0.0032(9) 569 À À O(7) 0.4720(4) 0.1273(3) 0.3959(2) 0.0201(5) 0.0162(11) 0.0222(11) 0.0213(11) 0.0021(9) À0.0032(8) À0.0056(9) O(8) 0.1909(5) À0.0929(2) 0.3600(3) 0.0200(5) 0.0214(11) 0.0144(10) 0.0247(11) 0.0054(8) À0.0042(9) À0.0035(8) O(9) 0.2710(5) 0.8701(3) 0.8935(3) 0.0247(5) 0.0160(11) 0.0356(14) 0.0218(11) 0.0014(10) 0.0006(9) À0.0026(10) O(10) 0.1377(6) 0.1631(3) 0.8947(3) 0.0310(6) 0.0298(14) 0.0305(14) 0.0333(14) 0.0064(11) À0.0013(11) À0.0092(11) O(11) 0.2305(5) 0.3942(3) 0.1149(3) 0.0275(5) 0.0221(12) 0.0312(14) 0.0300(13) 0.0056(11) 0.0039(10) 0.0012(10) O(12) 0.3467(6) 0.6878(3) 0.0819(3) 0.0313(6) 0.0354(15) 0.0309(14) 0.0270(13) 0.0018(11) À0.0031(11) 0.0095(12) H(1) 0.436(6) 0.912(7) 0.877(7) 0.084(8)* H(2) 0.203(12) 0.819(7) 0.805(4) 0.084(8)* H(3) 0.135(13) 0.260(3) 0.947(6) 0.084(8)* H(4) 0.112(13) 0.156(7) 0.793(1) 0.084(8)* H(5) 0.075(7) 0.449(6) 0.133(7) 0.084(8)* H(6) 0.273(13) 0.360(7) 0.205(4) 0.084(8)* H(7) 0.320(13) 0.764(5) 0.022(6) 0.084(8)* H(8) 0.420(12) 0.717(7) 0.176(3) 0.084(8)* * constrained to be equal duringrefinement F.
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    STRONG AND WEAK INTERLAYER INTERACTIONS OF TWO-DIMENSIONAL MATERIALS AND THEIR ASSEMBLIES Tyler William Farnsworth A dissertation submitted to the faculty at the University of North Carolina at Chapel Hill in partial fulfillment of the requirements for the degree of Doctor of Philosophy in the Department of Chemistry. Chapel Hill 2018 Approved by: Scott C. Warren James F. Cahoon Wei You Joanna M. Atkin Matthew K. Brennaman © 2018 Tyler William Farnsworth ALL RIGHTS RESERVED ii ABSTRACT Tyler William Farnsworth: Strong and weak interlayer interactions of two-dimensional materials and their assemblies (Under the direction of Scott C. Warren) The ability to control the properties of a macroscopic material through systematic modification of its component parts is a central theme in materials science. This concept is exemplified by the assembly of quantum dots into 3D solids, but the application of similar design principles to other quantum-confined systems, namely 2D materials, remains largely unexplored. Here I demonstrate that solution-processed 2D semiconductors retain their quantum-confined properties even when assembled into electrically conductive, thick films. Structural investigations show how this behavior is caused by turbostratic disorder and interlayer adsorbates, which weaken interlayer interactions and allow access to a quantum- confined but electronically coupled state. I generalize these findings to use a variety of 2D building blocks to create electrically conductive 3D solids with virtually any band gap. I next introduce a strategy for discovering new 2D materials. Previous efforts to identify novel 2D materials were limited to van der Waals layered materials, but I demonstrate that layered crystals with strong interlayer interactions can be exfoliated into few-layer or monolayer materials.
  • Gems and Minerals of Maine Pegmatites

    Gems and Minerals of Maine Pegmatites

    Gems and Minerals of Maine Pegmatites Carl A. Francis Granitic pegmatites in Maine have been collected, commercially mined, and scientifically investigated for two centuries. Feldspar is by far the most important commercial product, but it is the sporadic production of gemstones beginning in the 1820s and continuing to the present that sustains interest in exploring Maine's many pegmatites. The only other pegmatite district in North America with significant gem production is in San Diego County of southern California. In a review paper Wise and Francis (1992) using the scheme of Cerny (1982) classified Maine's pegmatites as "rare element" pegmatites and grouped them into two pegmatite "fields". The Brunswick field is located along the seacoast northeast of Portland. The Oxford field is inland northwest of Portland. A fault of regional significance separates the two terranes in which they are located. Both fields have been subdivided into clusters of pegmatites termed "series." The Brunswick field comprises four series of which the Topsham series is the most important and mineralogically interesting. It was the pioneering feldspar mining district in Maine. The Oxford field is much larger and comprises nine series. Cerny's model of pegmatite petrogenesis envisions a parent pluton of fertile granite surrounded by a fringe of daughter pegmatites with the pegmatites furthest from the pluton being the most enriched in rare elements. At least superficially the pegmatite series of the Oxford field corresponds to this model, whereas the Topsham series in the Brunswick field lacks an apparent parent. For this and other reasons the petrogenesis of Maine's pegmatites still cannot be considered well understood despite a century of study.
  • Atomic Minerals Contents

    Atomic Minerals Contents

    MA-SEM II ( CC- India Unit –I) Atomic Minerals Contents INTRODUCTION TO TOPIC Major Atomic Minerals in the World: 1.Uranium (U) 2. Thorium (Th) 3. Beryllium (Be) 4. Lithium (Li) 5. Zirconium (Zr) Conclusion Questions for Exams and Assignments References Learning Objectives: To understand the classification, distribution and Production and uses of atomic minerals in the World Learning Outcome: able to explain characteristics, uses, location and production of different atomic minerals. Keywords: Radioactive, Uranium, Thorium, Lithium, Beryllium INTRODUCTION Mineral is a naturally occurring inorganic substance, with fixed range in chemical composition, and is usually obtained by mining. Atomic minerals are the most important among non-fossil energy resources which are the minerals of radioactive elements like Uranium (U) and Thorium (Th). Atomic energy is produced by fission (splitting of the radioactive-elements like uranium) or by fusion (like colliding and fusing of two deuterons to form helium) of atomic nuclei, with matter being converted into energy in either process. Radioactivity was discovered in 1896 by the Henri Becquerel (1852-1908), Pierre and Marie Curie. Atomic Minerals are discrete minerals of Uranium and Thorium as uraninite (of U) and thorite (of Th). They also occur in notable quantity in mineral like of Rare Metals- Nobelium (Nb), Tantalum (Ta), Lithium (Li), Beryllium (Be), Zirconium- Zr, Sn, W etc). Atomic minerals are broadly divided in two groups- • 1. Primary minerals: Those are formed directly from magmas, hydrothermal Solution and groundwater. Example- Uraninite, Thorianite. • 2. Secondary minerals: These are formed due to remobilization of elements from primary minerals, their transportation in solution and later precipitation due to oversaturation in oxidizing or supergene environment.
  • THE 6Th INTERNATIONAL SYMPOSIUM on GRANITIC PEGMATITES

    THE 6Th INTERNATIONAL SYMPOSIUM on GRANITIC PEGMATITES

    CONTRIBUTIONS TO THE 6th INTERNATIONAL SYMPOSIUM ON GRANITIC PEGMATITES EDITORS WILLIAM B. SIMMONS KAREN L. WEBBER ALEXANDER U. FALSTER ENCARNACIÓN RODA-ROBLES SARAH L. HANSON MARÍA FLORENCIA MÁRQUEZ-ZAVALÍA MIGUEL ÁNGEL Galliski GUEST EDITORS ANDREW P. BOUDREAUX KIMBERLY T. CLARK MYLES M. FELCH KAREN L. MARCHAL LEAH R. GRASSI JON GUIDRY SUSANNA T. KREINIK C. MARK JOHNSON COVER DESIGN BY RAYMOND A. SPRAGUE PRINTED BY RUBELLITE PRESS, NEW ORLEANS, LA PEG 2013: The 6th International Symposium on Granitic Pegmatites PREFACE Phosphate Theme Session Dedicated to: François Fontan, André-Mathieu Fransolet and Paul Keller, It is a pleasure for the organizing committee to phosphates during the evolution of the pegmatites introduce the special session on phosphates, as an and on their relationship to other mineral phases, important part of the program of the 6th such as silicates. These kinds of studies are getting International Symposium on Granitic Pegmatites. more and more abundant, with some interesting The complexity of phosphate associations, examples in this volume. commonly occurring as a mixture of several fine- We take this opportunity to honor François grained phases, make their study difficult. However Fontan, Paul Keller and André-Mathieu Fransolet. over the last decades, the number of publications on These three exceptional researchers have pegmatite phosphate minerals has increased contributed enormously to the advancement in the exponentially as a result of new techniques. The knowledge on phosphates during the last decades. early investigations focused on description, They worked individually and jointly, always in an composition and paragenesis. Now that most of the enthusiastic, effective and tireless way. They passed phases have been extensively described and their knowledge and interest in phosphates onto replacement sequences of secondary phosphates are many younger researchers.