INORGANIC SYNTHESES Volume 35 - media control€¦ · Alison G. Barnes, Chemistry M313, School of...

INORGANIC SYNTHESES

Volume 35

.......

Board of Directors

THOMAS B. RAUCHFUSS, president University of Illinois at Urbana-Champaign

DIMITRI COUCOUVANIS University of Michigan

MARCETTAY. DARENSBOURG Texas A&M University

JOHN R. SHAPLEY University of Illinois at Urbana-Champaign

Secretary to the Corporation

STANTON CHING Connecticut College

Future Volumes

36 GREGORY S. GIROLAMI and ALFRED P. SATTELBERGER University of Illinois

at Urbana-Champaign and Argonne National Laboratory

37 PHILIP P. POWER University of California at Davis

International Associates

MARTIN A. BENNETT Australian National University

FAUSTO CALDERAZZO University of Pisa

M. L. H. GREEN Oxford University

JACK LEWIS Cambridge University

RENE POILBLANC University of Toulouse

HERBERT W. ROESKY University of Gottingen

WARREN R. ROPER University of Auckland

F. G. A. STONE Baylor University

JAN REEDIJK Leiden University

H. VAHRENKAMP University of Freiburg

AKIO YAMAMOTO Tokyo Institute of Technology

Editor-in-Chief

THOMAS B. RAUCHFUSS

University of Illinois at Urbana-Champaign

.................................................................

INORGANIC

SYNTHESES

Volume 35

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PREFACE

This volume presents procedures to compounds that illustrate the scope of modern

inorganic and organometallic synthesis. Following the tradition of Inorganic

Syntheses, emphasis has been placed on useful compounds and methods. Reflect-

ing my own interests, transition metal derivatives are featured.

The largest chapter concerns NacNac complexes. Such complexes represent

versatile platforms for a variety of transformations. The NacNac ligands have

many desirable features, not the least of which is the scope of their substituted

derivatives. The set of procedures was organized by three leaders in this area,

Professors Daniel J. Mindiola, Patrick L. Holland, and Timothy H. Warren. In

addition to their own contributions, they recruited other colleagues so that the

chapter consists of procedures for NacNac complexes of all metals from scandium

to zinc.

The remaining sections of the book reflect several areas of contemporary

activity. Routes are described to a selection of platinummetal reagents that straddle

the inorganic and organometallic domains, including some complexes that are of

interest in the area of solar energy research. A chapter highlights important

complexes from the area of bioorganometallic chemistry. We present an excellent

selection of electronically and stereochemically unusual ligands that are easily

prepared and adaptable to many metals, for example, the NHCs, bispidines, and

Kl€aui’s metalloligand. There is little question that metal-organic frameworks

(MOFs)will emerge as an important area of research and possibly applications.We

are fortunate to have detailed procedures for importantmembers of this new family

of molecule-based materials provided by the leading group in this area. As is our

tradition, the volume includes a series of procedures that do not neatly fit into any

category, such as salts of the remarkable radical [B12Me12]� and the hydrophilic

[B12(OH)12]2�. Finally, we include a collection of versatile classical coordination

and organometallic complexes.

Inorganic Syntheses has benefited from outstanding contributions from across

the globe, so I thank these authors and checkers first. Of the many people who

helped produce this volume, I wish to recognized my graduate and undergraduate

students, several ofwhom are listed as checkers.My colleaguesGregGirolami and

Scott Denmark were sources of advice and encouragement in this venture as they

have been throughout my career at Illinois. Finally, I wish to acknowledge the

previous editors of Inorganic Syntheses who have inspired me by their example.

v

The first chemistry monograph that I ever bought was Inorganic Syntheses,

Volume XIII, edited by F. A. Cotton.

I dedicate this volume to the memory of Alan M. Sargeson, a frequent

contributor to Inorganic Syntheses, inspired chemist, and gentleman.

THOMAS B. RAUCHFUSS

University of Illinois at Urbana-Champaign, Urbana, IL

vi Preface

CONTRIBUTORS

Debashis Adhikari, Department of Chemistry and Molecular Structure Center,

Indiana University, Bloomington, IN 47405

Enzo Alessio, Dipartimento di Scienze Chimiche, Universita di Trieste, 34127

Trieste, Italy

NicoleL.Armanasco,ChemistryM313, School ofBiomedical, Biomolecular and

Chemical Sciences, The University of Western Australia, Crawley, WA 6009,

Australia

YosraM.Badiei,Department of Chemistry, GeorgetownUniversity,Washington,

DC 20057-1227

Murray V. Baker, Chemistry M313, School of Biomedical, Biomolecular and


Australia

Alison G. Barnes, Chemistry M313, School of Biomedical, Biomolecular and


Australia

Stefan Bernhard, Department of Chemistry, Princeton University, Princeton, NJ

08544

Soledad Betanzos-Lara, Department of Chemistry, University of Warwick,

Coventry CV4 7AL, UK

Steven M. Bischof, The Scripps Energy Laboratories, The Scripps Research

Institute, Jupiter, FL 33458

Karen J. Blackmore, Department of Chemistry, University of California, Irvine,

CA 92697

Ioannis Bratsos,Dipartimento di Scienze Chimiche, Universita di Trieste, 34127

Trieste, Italy

David H. Brown, Chemistry M313, School of Biomedical, Biomolecular and


Australia

Gloria Sanchez Cabrera, Centro de Investigaciones Quımicas, Universidad

Autonoma del Estado de Hidalgo, Pachuca, Estado de Hidalgo 42184, Mexico

vii

Maria Caporali, Consiglio Nazionale delle Ricerche, Istituto di Chimica dei

CompostiOrganometallici (ICCOM-CNR),50019SestoFiorentino(Firenze), Italy

Chien-Hong Chen, School of Applied Chemistry, Chung Shan Medical Univer-

sity, Taichung, Taiwan

Anthony R. Chianese, Department of Chemistry, Yale University, New Haven,

CT, 06520-8107

Karen P. Chiang, Department of Chemistry, University of Rochester, Rochester,

NY 14627

Young Keun Chung,Department of Chemistry, Seoul National University, Seoul

151-742, Korea

Joshua R. Clayton, Department of Chemistry and Biochemistry, University of

Colorado, Boulder, CO 80309

Eric D. Cline, Department of Chemistry, Princeton University, Princeton, NJ

08544

Peter Comba, Anorganisch-Chemisches Institut, Universitat Heidelberg,

D-69120 Heidelberg, Germany

Timothy R. Cook, Department of Chemistry, Massachusetts Institute of Tech-

nology, Cambridge, MA 02139-4307

Ryan E. Cowley, Department of Chemistry, University of Rochester, Rochester,

NY 14627

Robert H. Crabtree,Department of Chemistry, Yale University, New Haven, CT

06520-8107

Keying Ding, Department of Chemistry, University of Rochester, Rochester, NY

14627

Anders Døssing,Department of Chemistry, University of Copenhagen, DK-2100

Copenhagen Ø, Denmark

Christos Douvris, Department of Chemistry and Biochemistry, University of


Daniel L. DuBois, Chemical and Materials Sciences Division, Pacific Northwest

National Laboratory, Richland, WA 99352

Mary Rakowski DuBois, Chemical and Materials Sciences Division, Pacific

Northwest National Laboratory, Richland, WA 99352

Lisa Dudek, Department of Chemistry and Biochemistry, University of

California, Los Angeles, CA 90095-1569

viii Contributors

ThomasR.Dugan,Department of Chemistry, University ofRochester, Rochester,

NY 14627

Celine Fellay, Institut des Sciences et Ingenierie Chimiques, Ecole Polytechnique

Federale de Lausanne (EPFL), CH-1015 Lausanne, Switzerland

Matthew G. Fete, Department of Chemistry and Biochemistry, University of


Anne Mette Frey, Department of Chemistry, University of Copenhagen, DK-

2100 Copenhagen Ø, Denmark

Benjamin R. Garrett,Department of Chemistry, University of Illinois at Urbana-

Champaign, Urbana, IL 61801

Starla D. Glover, Department of Chemistry and Biochemistry, University of

California at San Diego, San Diego, CA 92093

John C. Goeltz, Department of Chemistry and Biochemistry, University of


Luca Gonsalvi, Consiglio Nazionale delle Ricerche, Istituto di Chimica dei

Composti Organometallici (ICCOM-CNR), 50019 Sesto Fiorentino (Firenze),

Italy

Abraha Habtemariam, Department of Chemistry, University of Warwick, Cov-

entry CV4 7AL, UK

James Hauk, Department of Chemistry and Biochemistry, University of


M. Frederick Hawthorne, International Institute of Nano and Molecular Medi-

cine, University of Missouri, Columbia, MO 65211

Paul G. Hayes, Department of Chemistry and Biochemistry, University of

Lethbridge, Lethbridge, Alberta, Canada T1K 3M4

Valerie J. Hesler, Chemistry M313, School of Biomedical, Biomolecular and


Australia

Alan F. Heyduk, Department of Chemistry, University of California, Irvine, CA

92697

YutakaHitomi,Department ofMolecular Chemistry andBiochemistry, Doshisha

University, Kyotanabe, Kyoto 610-0321, Japan

Patrick L. Holland, Department of Chemistry, University of Rochester,

Rochester, NY 14627

Contributors ix

Maik Jakob,Anorganisch-Chemisches Institut, Universitat Heidelberg, D-69120

Heidelberg, Germany

Satish S. Jalisatgi, International Institute of Nano and Molecular Medicine,

University of Missouri, Columbia, MO 65211

Yuuji Kajita, Department of Molecular Chemistry and Biochemistry, Doshisha

University, Kyotanabe, Kyoto 610-0321, Japan

Marion Kerscher, Anorganisch-Chemisches Institut, Universitat Heidelberg,

D-69120 Heidelberg, Germany

SangBokKim,Department ofChemistry, BrownUniversity, Providence, RI 02912

Benjamin T. King, Department of Chemistry and Biochemistry, University of


Yoshihisa Kishima, Department of Molecular Chemistry and Biochemistry,

Doshisha University, Kyotanabe, Kyoto 610-0321, Japan

Wolfgang Klaui, Lehrstuhl I: Bioanorganische Chemie und Katalyse, Heinrich-

Heine-Universitat Dusseldorf, 40225 Dusseldorf, Germany

Masahito Kodera, Department of Molecular Chemistry and Biochemistry,


Elzbieta Kogut, Department of Chemistry, Georgetown University, Washington,

DC 20057-1227

Clifford P. Kubiak, Department of Chemistry, University of California at San

Diego, San Diego, CA 61801

Peter C. Kunz, Lehrstuhl I: Bioanorganische Chemie und Katalyse, Heinrich-

Heine-Universitat Dusseldorf, 40225 Dusseldorf, Germany

Gabor Laurenczy, Institut des Sciences et Ingenierie Chimiques, Ecole Poly-

technique Federale de Lausanne (EPFL), CH-1015 Lausanne, Switzerland

Mark W. Lee, Jr., International Institute of Nano and Molecular Medicine,


Christopher S. Letko,Department of Chemistry, University of Illinois at Urbana-


Chin Hin Leung, Department of Chemistry, Yale University, New Haven, CT

06520-8107

Wen-Feng Liaw, Department of Chemistry, National Tsing Hua University,

Hsinchu 30043, Taiwan

x Contributors

Simon Lotz, Department of Chemistry, University of Pretoria, Pretoria 0002,

South Africa

Leonard A.MacAdams,Department of Chemistry and Biochemistry, University

of Delaware, Newark, DE 19716

Amanda E. Mack, Department of Chemistry, University of Illinois at Urbana-


Neal D.McDaniel,Department of Chemistry, Princeton University, Princeton, NJ

08544

Marie M. Melzer, Department of Chemistry, Georgetown University, Washing-

ton, DC 20057-1227

JosefMichl,Department of Chemistry and Biochemistry, University of Colorado,

Boulder, CO 80309; Institute of Organic Chemistry and Biochemistry, Academy

of Sciences of the Czech Republic, 16610 Prague 6, Czech Republic

Daniel J. Mindiola, Department of Chemistry and Molecular Structure Center,

Indiana University, Bloomington, IN 47405

Tomoyuki Nakagawa, Department of Molecular Chemistry and Biochemistry,


Andy I. Nguyen, Department of Chemistry, University of California, Irvine, CA

92697

Daniel G. Nocera, Department of Chemistry, Massachusetts Institute of Tech-

nology, Cambridge, MA 02139-4307

Michael R. North, Chemistry M313, School of Biomedical, Biomolecular and


Australia

Yasuhiro Ohki, Department of Chemistry, Graduate School of Science, and

Research center for Materials science, Nagoya University, Nagoya 464-8602,

Japan

Shun Ohta,Department of Chemistry, Graduate School of Science, and Research

center for Materials science, Nagoya University, Nagoya 464-8602, Japan

RoyA.Periana,TheScripps EnergyLaboratories, TheScrippsResearch Institute,

Jupiter, FL 33458

Maurizio Peruzzini, Consiglio Nazionale delle Ricerche, Istituto di Chimica dei


Italy

Contributors xi

Warren E. Piers, Department of Chemistry, University of Calgary, Calgary,

Alberta, Canada T2N 1N4

Robert D. Pike, Department of Chemistry, College of William and Mary,

Williamsburg, VA 23187

Chuleeporn Puttnual,Department of Chemistry and Biochemistry, University of

Delaware, Newark, DE 19716

Udo Radius, Institut fur Anorganische Chemie der Universitat Wurzburg, 97074

Wurzburg, Germany

Thomas B. Rauchfuss, Department of Chemistry, University of Illinois at

Urbana-Champaign, Urbana, IL 61801

Herbert W. Roesky, Institut fur Anorganische Chemie, Universitat Gottingen,

D-37077 Gottingen, Germany

D. Ruckerbauer, Institute of Chemistry, Inorganic Department, Karl-Franzens-

University, 8010 Graz, Austria

Peter J. Sadler,Department of Chemistry, University ofWarwick, Coventry CV4

7AL, UK

Alexander V. Safronov, International Institute of Nano andMolecular Medicine,


Thomas Schaub, BASF SE, 67056 Ludwigshafen, Germany

Bryan D. Stubbert, Department of Chemistry, University of Rochester,

Rochester, NY 14627

Shouheng Sun, Department of Chemistry, Brown University, Providence, RI

02912

DwightA. Sweigart,Department of Chemistry, BrownUniversity, Providence, RI

02912

Yoshimitsu Tachi, Department of Molecular Chemistry and Biochemistry,


Kazuyuki Tatsumi, Department of Chemistry, Graduate School of Science, and

Research Center for Materials Science, Nagoya University, Nagoya 464-8602,

Japan

Thomas S. Teets, Department of Chemistry, Massachusetts Institute of Technol-

ogy, Cambridge, MA 02139-4307

Klaus H. Theopold, Department of Chemistry and Biochemistry, University of

Delaware, Newark, DE 19716

xii Contributors

Leonard L. Tinker, Department of Chemistry, Princeton University, Princeton,

NJ 08544

Ba L. Tran, Department of Chemistry and Molecular Structure Center, Indiana

University, Bloomington, IN 47405

David J. Tranchemontagne, Department of Chemistry and Biochemistry, Uni-

versity of California, Los Angeles, CA 90095-1569

Michal Valasek, Institute of Organic Chemistry and Biochemistry, Academy of

Sciences of the Czech Republic, 16610 Prague 6, Czech Republic

Matthew S. Varonka, Department of Chemistry, Georgetown University,

Washington, DC 20057-1227

Victoria Volkis, Department of Chemistry and Biochemistry, University of


AdelinaM. Voutchkova,Department of Chemistry, Yale University, NewHaven,

CT 06520-8107

Timothy H. Warren, Department of Chemistry, Georgetown University,

Washington, DC 20057-1227

J. W. Wielandt, Institute of Chemistry, Inorganic Department, Karl-Franzens-

University, 8010 Graz, Austria

Stefan Wiese, Department of Chemistry, Georgetown University, Washington,

DC 20057-1227

Omar M. Yaghi, Department of Chemistry and Biochemistry, University of

California, Los Angeles, CA 90095-1569

Fabrizio Zanobini, Consiglio Nazionale delle Ricerche, Istituto di Chimica dei


Italy

IlyaZharov,Department of Chemistry andBiochemistry, University of Colorado,

Boulder, CO 80309

Francisco J. Zuno-Cruz, Centro de Investigaciones Quımicas, Universidad

Autonoma del Estado de Hidalgo, Pachuca, Estado de Hidalgo 42184, Mexico

Contributors xiii

DEDICATION

This volume is dedicated to the memory of four eminent chemists who made

outstanding contributions to inorganic chemistry in general and to Inorganic

Syntheses in particular. We mourn their passing, but we celebrate their

achievements.

ROBERT W. PARRY (EDITOR-IN-CHIEF, VOLUME XII, 1970)

Bob was born on October 1, 1917 in Ogden, UT, and died on December 1, 2006 in

Salt Lake City, UT, at the age of 89, following a stroke. He received his B.S. degree

in soil chemistry fromUtah StateAgricultural College (nowUtah StateUniversity)

(1940), his M.S. degree in soil chemistry from Cornell University (1942), and his

Ph.D. in inorganic coordination chemistry under John C. Bailar, Jr. (Editor-in-

Chief, Inorganic Syntheses, Volume IV, 1953) from the University of Illinois

(1946). He served on the chemistry faculties of the University of Michigan

(1946–1969) and the University of Utah (Distinguished Professor of Chemistry,

1969–1997).

An extraordinary teacher, Bob coauthored the widely used high school text,

Chemistry: Experimental Foundations (1970), was senior author of Prentice-

Hall’s high school chemistry curriculum program (CHEM STUDY), and was

coeditor of Prentice-Hall’s paperback series, Foundations of General Chemistry.

He mentored more than 60 Ph.D. students and postdoctoral fellows. His honors

include first recipient of the ACS Award for Distinguished Service in Inorganic

Chemistry (1965), Manufacturing Chemists Award for Excellence in the Teaching

of College Chemistry (1972), ACS Award in Chemical Education (1977),

Alexander von Humboldt Senior U.S. Scientist Award (1980, 1983), first State

of Utah Governor’sMedal in Science and Technology (1987), honorary doctorates

from the Utah State University (1985) and the University of Utah (1997), and the

ACS’s highest honor, the Priestley Medal (1993).

Bob authored more than 150 publications, not only on the boron hydrides but

also on gallium, phosphines, and the thermodynamics of chelation. Long active in

the ACS, he served as President (1982), member of the Council for more than 45

years and of the Board of Directors (1973–1983), and Associate Editor of the

Journal of the American Chemical Society (1966–1968, 1971–1980), and a

member of its Editorial Board (1969–1980). He was the founding editor of

Inorganic Chemistry (1960–1964) and a member of its Editorial Board

(1962–1979) and President of Inorganic Syntheses, Inc. (1969–1972). One of the

early leaders of the Gordon Research Conferences, hewas a member (1965–1972)

xv

and Chairman (1967–1968) of the GRC Board of Trustees. He was Executive

Secretary, Chairman, and Councilor of the American Association for the Ad-

vancement of Science between 1980 and 1995, and he held offices in the

International Union of Pure and Applied Chemistry between 1965 and 1982.

FRANK ALBERT COTTON (EDITOR-IN-CHIEF, VOLUME XIII, 1973)

Al, one of the twentieth century’smost prolific, creative, and influential inorganic

chemists and chemical educators, was born on April 9, 1930 in Philadelphia, PA,

and died following a violent attack on February 20, 2007 in College Station, TX,

at the age of 76. He received his primary, secondary, and undergraduate education

in Philadelphia, enrolling in the Drexel Institute of Technology, intending to

major in chemical engineering. He switched to chemistry and received his B.S.

degree from Temple University (1951). He began graduate study at Harvard

University, where he joined the research group of future (1973) Nobel chemistry

laureate Geoffrey Wilkinson and worked on ferrocene and other metallocenes.

After receiving his Ph.D. (1955), he became an Instructor at the Massachusetts

Institute of Technology. In 1961, at the age of 3l, he became MIT’s youngest full

Professor.

As one of the small number of chemists credited with initiating the renaissance

of inorganic chemistry that began in the 1950s, Al researched metal carbonyls,

ligand field theory, organometallic compounds, phosphine oxide and sulfide

complexes, metal complexes with high coordination numbers, protein X-ray

crystallography, fluxional organometallic molecules, and application of such

physicochemical techniques as infrared and ultraviolet spectroscopies to transition

metal complexes. His synthesis and characterization of the [Re2Cl8]� (1964)

opened a new field of research in multiple metal-metal bonds, metal clusters, and

extended solids. He proposed the hapto (h) nomenclature to indicate the structures

of p-bonded hydrocarbon ligands.

In 1971, Al became Robert A. Welch Professor of Chemistry and shortly

thereafter W. T. Doherty-Welch Distinguished Professor of Chemistry at Texas

A&M University, where he worked on the synthesis and characterization of

compounds with multiple and/or single metal–metal bonds and other unusual

species. He and his 118 Ph.D. students and more than 150 postdoctoral fellows

from over 30 countries produced more than 1600 publications. He was an ardent

and articulate advocate of ‘‘curiosity-driven’’ basic research.

Al received many awards from American and foreign societies, including the

U.S. National Medal of Science (1982), Robert A. Welch Award (1994), and

Israel’s Wolf Prize (2000). His major ACS honors include the Award in Inorganic

Chemistry (first recipient, 1962), Award for Distinguished Service in the Ad-

vancement of Inorganic Chemistry (1974), Award in Organometallic Chemistry

(2001), F. Albert Cotton Medal for Excellence in Chemical Research (first

recipient, 1995), George C. Pimentel Award in Chemical Education (2005), and

xvi Dedication

the ACS’s highest award, the Priestley Medal (1998). The ACS’s F. Albert Cotton

Award in Synthetic Inorganic Chemistry bears his name. He also received 29

honorary doctorates from universities around the world.

Al was a prominent scientific educator and textbook author. His Advanced

Inorganic Chemistry, coauthoredwith GeoffWilkinson, became a standard text. It

underwent six editions (1962–1999), sold more than half a million copies, and was

translated into 15 foreign languages. From his lecture notes, he wrote Chemical

Applications of Group Theory (1963, 1971, 1990). His Chemistry—An Investiga-

tive Approach (1973, 1976) was intended for high schools, and hisBasic Inorganic

Chemistry (1976, 1987, 1995) was an entry-level text.

FRED BASOLO (EDITOR-IN-CHIEF, VOLUME XVI, 1976)

Fredwas born of Italian immigrant parents on February 11, 1920 in Coello, a small

coal mining town in southern Illinois, and died on February 27, 2007 in Skokie, IL,

at the age of 87. Until he attended school, he spoke the Piedmontese dialect,

understanding but speaking little English. The first Coello resident to attend

college, he earned his B.Ed, degree from Southern Illinois Normal School (now

Southern Illinois University) (1940), intending to teach high school. However, he

pursued graduate studies at the University of Illinois on platinum complexes under

John C. Bailar, Jr. (Editor-in-Chief, Inorganic Syntheses, Volume IV, 1953),

earning his M.S. (1942) and Ph.D. (1943) degrees. After 3 years of war-related

research at Rohm and Haas near Philadelphia, PA, he joined the faculty of

Northwestern University as Instructor. He rose through the ranks, becoming

Charles E. and Emma H. Morrison Professor of Chemistry (1980–1990). He

served as Chairman of the Chemistry Department (1969–1972).

Fred realized that thework on kinetics andmechanisms of substitution reactions

on carbon being investigated by organic chemists could be applied to inorganic

coordination compounds such as those of cobalt(III) and platinum(II). He con-

vinced his colleagueRalphG. Pearson to join him in such studies, and the two soon

became leaders in the field, and their monograph, Mechanisms of Inorganic

Reactions (1958, 1967), became a classic. Their postulation of a SN1CB mecha-

nism for the base hydrolysis of cobalt(III) complexes led to a controversy with

Christopher K. Ingold and Ronald S. Nyholm that was resolved in Basolo and

Pearson’s favor and garnered them and Northwestern University a global

reputation.

Fred maintained an international perspective, spending sabbatical leaves

with Jannik Bjerrum (1954–1955) and Vincenzo Caglioti (1961–1962). He

regarded Italy as a second home and was elected to the Accademia Nazionale

dei Lincei (1987), the world’s oldest scientific society. He coauthored Coordi-

nation Chemistry (1964, 1986) with former student Ronald C. Johnson.

Fred cofounded the Inorganic Gordon Research Conference, which continues

today.

Dedication xvii

In the ACS, Fred was elected Chairman of the Division of Inorganic Chemistry

(1970), a member of its Executive Committee, and President of the society (1983).

He received the following ACS honors—Award in Inorganic Chemistry (1964),

Award for Distinguished Service in the Advancement of Inorganic Chemistry

(1975), George C. Pimentel Award in Chemical Education (1993), and the

Priestley Medal, the society’s highest honor (2001).

ALAN G. MACDIARMID (EDITOR-IN-CHIEF, VOLUME XVII, 1977)

Alan was born onApril 14, 1927 inMasterton, NewZealand, and died on February

7, 2007 in Philadelphia, PA, after falling in his home. His youth was spent in

poverty (his father lost his job because of the Great Depression), and he left high

school at the age of 16 to help support the family. As a part-time student with a low-

paying ‘‘lab boy’’ (janitor) job in the Chemistry Department of Victoria University

College at Wellington, he earned his B.Sc. degree (1947) and then became a

demonstrator and worked as an assistant. His first publication (in Nature, 1949)

dealt with S4N4, a molecule that played a role in his later Nobel-winning research.

After graduating with a M.Sc. degree with first class honors (1951), Alan

received a Fulbright Fellowship that enabled him to study the rate of exchange in14C-tagged metal cyanide complexes at the University of Wisconsin, Madison,

from which he received his M.S. (1952) and Ph.D. (1953) degrees. With a New

Zealand Shell graduate scholarship, he then studied silicon hydrides underHarry J.

Emel�eus at Cambridge University, earning his second Ph.D. degree (1955).

Following short stints at Queen’s College and the University of St. Andrews, he

joined the Department of Chemistry at the University of Pennsylvania, where he

spent the remainder of his career, rising through the ranks and becomingBlanchard

Professor of Chemistry (1988). In 2002, he became James Von Ehr Distinguished

Professor of Science & Technology at the University of Texas, Dallas.

After devoting himself to silicon chemistry for two decades, Alan began a

fruitful collaborationwith his colleagueAlan J.Heeger on the conducting polymer,

(SN)x, the precursor to which he had studied in Wellington. While a Visiting

Professor at Kyoto University, Alan visited the Tokyo Institute of Technology,

where Hideki Shirakawa showed him a silvery film of polyacetylene. Shirakawa

accepted Alan’s invitation to spend a year with him studying this substance. They

discovered that the impurity in polyacetylene served as a dopant and increased its

conductivity. By adding bromine to the (CH)x films, they increased the conduc-

tivity by many millions of times. The two collaborated with Heeger, and in 2000

the trio shared theNobel Prize inChemistry ‘‘for the discovery and development of

conductive polymers.’’ Alan wrote more than 600 articles and held 20 patents. His

honors include the ACS’s Frederic Stanley Kipping Award in Silicon Chemistry

(1971) and Award in the Chemistry ofMaterials (1999); the RutherfordMedal, the

Royal Society of New Zealand’s highest honor (2000); election to the U.S.

NationalAcademyof Sciences (2002) and theOrder ofNewZealand, the country’s

xviii Dedication

highest honor (2002); and the fellowship in the Royal Society (2003). His alma

mater, Victoria University, awarded him an honorary doctorate (1999), created a

chair in physical chemistry in his name (2001), and named an Institute for

Advanced Materials and Nanotechnology after him (2003). Institutes named after

him include those at Jilin University in China (2001) and the University of Texas,

Dallas (2007).

STANLEY KIRSCHNER (EDITOR-IN-CHIEF, VOLUME XXIII, 1985)

Stan was born on December 17, 1927 in Brooklyn, New York and died on July 16,

2008. Stan attended New York City’s renowned Stuyvesant High School. He had

decided on a career in chemistry after his father, a pharmacist, presented himwith a

chemistry set when he was 11 years old.

After graduation Stan enlisted in the U.S. Navy (1944–1945), but then attended

Brooklyn College, from which he received his B.S. degree in 1950. Following a

brief stint with theMonsanto Chemical Company, he attendedHarvard University,

where hewon a departmental award as the best teaching fellow and fromwhich he

received his A.M. degree in 1952. He studied inorganic chemistry at theUniversity

of Illinois under John C. Bailar, Jr. (one of the founders of Inorganic Syntheses and

Editor-in-Chief of Volume 4, 1953). After receiving his Ph.D. in 1954, Stan joined

the faculty of Wayne State University in Detroit, Michigan, where he spent his

entire career, rising through the ranks and retiring as Professor Emeritus in 1992.

Stan was a longtime Secretary of the Editorial Board of Inorganic Syntheses.

His awards and honors include the Wayne State University President’s Award for

Excellence in Teaching (1969), Heyrovsk�y Medal of the Czechoslovak Academy

of Sciences (1978), the ACS Detroit Section’s Distinguished Service Award

(1980), the ChemicalManufacturers Award for Excellence in Chemistry Teaching

(1984), and the ACS Henry Hill Award and Engineering Society of Detroit’s Gold

Award (both in 1995),

Stan’s some one hundred articles dealt with the synthesis, structure, stereo-

chemistry, and biological properties of coordination compounds, including the

anticancer activity of platinum complexes; optical rotatory dispersion; circular

dichroism; the Pfeiffer Effect inmetal complexes; inorganic nomenclature; and the

application of computer techniques to chemical and information problems. A

prominent educator, he edited three books on inorganic and coordination

chemistry.

Because of his ebullient personality, organizational talent, and interest in

foreign languages, Stan held visiting professorships and similar honorary appoint-

ments across the globe. Among his many positions, he held positions at University

College, London (with Ronald S. Nyholm), University of S~ao Paolo in Brazil, theCentrul de Chimie in Timisoara and Institutul de Chimie in Cluj-Napoca in

Romania; the University of Florence, Tohoku University, and both the Technical

University and the University of Porto in Portugal. He held honorary membership

Dedication xix

in the national societies of most of these countries. Stan was an omnipresent

participant at the International Conference on Coordination Chemistry, the longest

running conference dedicated to inorganic chemistry. He attended every meeting

from 1959 to 2002 and serving as Permanent Secretary and Permanent Secretary

Emeritus.

GEORGE B. KAUFFMAN

California State University, Fresno, CA

xx Dedication

NOTICE TO CONTRIBUTORSAND CHECKERS

The Inorganic Syntheses series is published to provide all users of inorganic

substances with detailed and reliable procedures for the preparation of important

and timely compounds. Thus, the series is the concern of the entire scientific

community. The Editorial Board hopes that many chemists will share in the

responsibility of producing Inorganic Syntheses by offering their advice and

assistance in both the formulation and the laboratory evaluation of outstanding

syntheses. Help of this kind will be invaluable in achieving excellence and

pertinence to current scientific interests.

There is no rigid definition of what constitutes a suitable synthesis. The major

criterion by which syntheses are judged is the potential value to the scientific

community. An ideal synthesis is one that presents a new or revised experimental

procedure applicable to a variety of related compounds, at least one of which is

critically important in current research. Syntheses of individual compounds that

are of interest or importance are, however, also acceptable. Syntheses of com-

pounds that are readily available commercially at reasonable prices are ordinarily

not acceptable. Corrections and improvements of syntheses already appearing in

Inorganic Syntheses are suitable for inclusion.

The Editorial Board lists the following criteria of content for submitted

manuscripts. Style should conform with that of previous volumes of Inorganic

Syntheses. The introductory section should include a concise and critical summary

of the available procedures for synthesis of the product in question. It should also

include an estimate of the time required for the synthesis, an indication of the

importance and utility of the product, and an admonition if any potential hazards

are associated with the procedure. The Procedure section should present detailed

and unambiguous laboratory directions and bewritten so that it anticipates possible

mistakes and misunderstandings on the part of the person who attempts to

duplicate the procedure. Unusual equipment or procedure should be clearly

described. Line drawings should be included when they can be helpful. Safety

measures should be stated clearly. Sources of unusual starting materials must be

given, and, if possible, minimal standards of purity of reagents and solvents should

be stated. The scale should be reasonable for normal laboratory operation, and

problems involved in scaling the procedure either up or down should be discussed.

The criteria for judging the purity of the final product should be delineated clearly.

The Properties section should supply and discuss those physical and chemical

characteristics that are relevant to judging the purity of the product and to

xxi

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