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The Crystal and Molecular Structure of Tris(Ortho- Aminobenzoato)Aquoyttrium(Iii)

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The Crystal and Molecular Structure of Tris(Ortho- Aminobenzoato)Aquoyttrium(Iii) University of New Hampshire University of New Hampshire Scholars' Repository Doctoral Dissertations Student Scholarship Fall 1979 THE CRYSTAL AND MOLECULAR STRUCTURE OF TRIS(ORTHO- AMINOBENZOATO)AQUOYTTRIUM(III) SHARON MARTIN BOUDREAU Follow this and additional works at: https://scholars.unh.edu/dissertation Recommended Citation BOUDREAU, SHARON MARTIN, "THE CRYSTAL AND MOLECULAR STRUCTURE OF TRIS(ORTHO- AMINOBENZOATO)AQUOYTTRIUM(III)" (1979). Doctoral Dissertations. 1228. https://scholars.unh.edu/dissertation/1228 This Dissertation is brought to you for free and open access by the Student Scholarship at University of New Hampshire Scholars' Repository. It has been accepted for inclusion in Doctoral Dissertations by an authorized administrator of University of New Hampshire Scholars' Repository. For more information, please contact [email protected]. 8009658 Bo u d r e a u , S h a r o n M a r t in THE CRYSTAL AND MOLECULAR STRUCTURE OF TRIS(ORTHO- AMrNOBENZOATO)AQUOYTTRIUM(III) University o f New Hampshire PH.D. 1979 University Microfilms International 300 N. Zeeb Road, Ann Arbor, MI 48106 18 Bedford Row, London WC1R 4EJ, England PLEASE NOTE: In all cases this material has been filmed in the best possible way from the available copy. Problems encountered with this document have been identified here with a check mark . 1. Glossy photographs _ / 2. Colored illustrations _______ 3. Photographs with dark background \/ '4. Illustrations are poor copy 5. Print shows through as there is text on both sides of page ________ 6. Indistinct, broken or small print on several pages \/ throughout 7. Tightly bound copy with print lost in spine 8. Computer printout pages with indistinct print 9. Page(s) lacking when material received, and not available from school or author _______ 10. Page(s) _______ seem to be missing in numbering only as text follows _______ 11. Poor carbon copy _______ 12. Not original copy, several pages with blurred type 13. Appendix pages are poor copy ________ 14. Original copy with light type ________ 15. Curling and wrinkled pages _______ 16. Other University M icrailm s Irternarjonal 300 N ZEES RD.. ANN AR30R Ml J8106 '313) 761-4700 THE CRYSTAL AND MOLECULAR STRUCTURE OF TRIS( ORTHO-AMINOBENZOATO)AQUOYTTRIUM( I I I ) Ly SHARON MARTIN BOUDREAU B.A. , Wheaton College Norton, Massachusetts, 1975 A DISSERTATION Submitted to the University of New Hampshire In Partial Fulfillment of The Requirements for the Degree of DOCTOR OF PHILOSOPHY in C hem istry September, 1979 ; This thesis has been examined and approved. O — t — 4 Helmut M. Haendler, Thesis Director Professor of Chemistry C. L. Grant Professor of Chemistry • y y i f j v Y w ^ Jamek D. M o rriso n B^jfessor of Chemistry C h a rle s W. Owens Professor of Chemistry M. Wayne M y B easley U Associate Professor of M aterials Science / ? 7 y TO MY HUSBAND, PARENTS, AND FAMILY who, through their love and support, made this thesis possible Ac knowledgeme nts The author wishes to express her sincere appreciation to her research director, Dr. Helmut M. Haendler, for his guidance, support, and friendship during the course of this research and for the opportunity to share a unique learning experience. Gratitude is expressed to Dr. C.L. Grant and the faculty of the Department of Chemistry for providing the opportunities to teach chemistry. The experience of teaching was very important in the professional development of the author.. In addition, thanks is extended to my father whose own chemistry background set the stage for my career, and to my mother for her never ending love and encouragement. The author is grateful for the financial assistance of the Lester Eratt Fellowship, two University of New Hampshire Summer Fellowships, Dissertation Year Fellowship, and teaching assistantships. TABLE OF CONTENTS List of Tables .................................................................................................................... v i i List of Figures • • viii A b s tra c t ....................... ........................................................................................... ix The Crystal and Molecular Structure of Trisfortho-aminobenzoato)aquoyttrium(III) P a r t One The Synthesis of Metal Complexes of Ortho-aminobenzoic Acid ............ 1 I. Introduction ....................................................................................................... 1 II. Experimental ....................................................................................................... 7 A. S t a r t in g M a te ria ls .......................... 7 B. Preparation of Sodium Ortho-aminobenzoate Reagent ............... 7 C. Preparation of Metal Anthranilates ............................................... 7 D. Preparation of Single Crystals of Cadmium(ll), Cobalt(ll), Zinc(ll), Y ttrium (lll), and Lanthanum(lll) Anthranilates 8 E. X-Ray Powder Diffraction Patterns ................................................. 11 F. Elemental Analyses ....................................................... 11 1. Carbon, Hydrogen, and N itrogen ................................................ 11 2. Determination of Yttrium and Lanthanum ................................... 11 G. Determination of the Existence of Coordinated Water Molecules in Zn(ll), Y (lll), and La(lll) Anthranilates .. 12 III. Results and Discussion ......................................................................... 13 A. Single Crystal Growth ............................................................................. 13 B. Characterization of the Compounds ................................................ 17 C. Suggested Future Research .................................................................... 18 v P a r t Two The Crystal and Molecular Structure of Tris(ortho-aminobenzoato) a q u o y ttr iu m ( lll) , YtHgNCgH^COO)^ • HgO ............................................................... 20 I. Introduction ............................................................................................................... 21 A. Coordination Number Six .......................................................................... 23 B. Coordination Number Seven ..................................................................... 23 1. Capped Trigonal Prism ...................................................................... 24 2. Capped Octahedron ................................................................................. 27 C. Coordination Number Eight ........... ................................................................. 28 1. Square Antiprism ................................................................................... 28 2. Dodecahedron ............................................................................................... 28 D. C o o rd in a tio n Number Nine ........................................................................ 29 E. Higher Coordination Numbers ............................................................ 30 II. Experimental ........................................................................................................... 31 A. Preparation of Single Crystals of Tris(ortho-aminobenzoato) aquoyttrium( III) ....................................................... 31 B. Determination of the Space Group, Unit Cell Dimensions, and Density of Tris(ortho-aminobenzoato)aquoyttrium(III) ............. 31 C. Intensity Measurements .......................................................................... 33 III. Solution and Refinement of the Structure ........... 43 IV. Results and Discussion .................................................................................. 65 Appendix ............................................................................................................................... 87 A. X-Ray Powder Diffraction Patterns ................................................... 88 B. Computer Programs ........................................................................................ 96 Bibliography ...................................................................................................................... 104 LIST OF TABLES I. Synthesized Metal Complexes of Ortho-aminobenzoic A cid .............16 II. Crystal Data for Y^NCgH^COO)^ • H20 .................................................36 III. Outline of the Structure Determination for a Compound Containing a Heavy Atom ..................................................................................44 IV. Co-ordinates of Equivalent Positions for Space Group, C2/c..4? V. Selected Patterson Map Peak Heights and Locations .......................49 VI. Final Positional and Thermal Parameters for y( h2mc6h |>coo)3 ■ h20 ............................................................................................................... 57 VII. Summary of Refinement Stages ........................................................................62 VIII. Calculated and Observed Structure Factors f o r Y(H2NC6H^C00 )3 ■ HgO ..................................................... 63 IX. Characteristic Parameters of the Coordination Polyhedron ...7 1 X. Bond Distances and Angles in Y(H 2NG^H^C00)3 ■ HgO........................77 XI. X-Ray Powder Diffraction Data for Zn(H 2NC^H^C00)2 ................... 89 XII. X-Ray Powder Diffraction Data for Y(H 2NC^H^C00)3 • K^O 90 XIII. X-Ray Powder Diffraction Data for La(H 2NC^H^C00)3 ......................91 XIV. X-Ray Powder Diffraction Data for Mn(H 2NC^H^C00)2 .......... 9 2 XV. X-Ray Powder Diffraction Data for Co(H 2NC^H^C00)2
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