Inorganic Syntheses, Volume 36

334 Pages·2014·1.784 MB·English

by  Gregory S. Girolami (ed.)

Editors-in-Chief
GREGORY S. GIROLAMI
University of Illinois at Urbana-Champaign
ALFRED P. SATTELBERGER
Argonne National Laboratory

INORGANIC
SYNTHESES
Volume 36

INORGANIC SYNTHESES
Volume 36
(cid:129)(cid:129)(cid:129)(cid:129)(cid:129)(cid:129)(cid:129)
BoardofDirectors
THOMASB.RAUCHFUSS,President UniversityofIllinoisatUrbana-Champaign
MARCETTAY.DARENSBOURG TexasA&MUniversity
GREGORYS.GIROLAMI UniversityofIllinoisatUrbana-Champaign
ALFREDP.SATTELBERGER ArgonneNationalLaboratory
JOHNR.SHAPLEY UniversityofIllinoisatUrbana-Champaign
SecretarytotheCorporation
STANTONCHING ConnecticutCollege
FutureVolumes
37PHILIPP.POWER UniversityofCaliforniaatDavis
InternationalAssociates
MARTINA.BENNETT AustralianNationalUniversity
MALCOLML.H.GREEN OxfordUniversity
JANREEDIJK LeidenUniversity
HERBERTW.ROESKY UniversityofGöttingen
WARRENR.ROPER UniversityofAuckland
Editors-in-Chief
GREGORY S. GIROLAMI
University of Illinois at Urbana-Champaign
ALFRED P. SATTELBERGER
Argonne National Laboratory

INORGANIC
SYNTHESES
Volume 36
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PREFACE
This volume of Inorganic Syntheses spans the preparations of a wide range of
important inorganic, organometallic, and solid-state compounds. Continuing a
long-standing tradition, we have emphasized useful compounds and methods.
Reflectingourownpersonalresearchinterests,transitionmetalhalides,complexes
with cyclopentadienyl and substituted cyclopentadienyl ligands, and compounds
with metal–metal bonds are featured. We have also included a chapter on
pedagogically important compounds that we hope will find their way into
undergraduate inorganic chemistry teaching laboratories.
The volume is divided into six chapters. Chapter 1 contains the syntheses of
some key early transition metal halide clusters and the very useful mononuclear
molybdenum(III)synthon,MoCl (THF) .Thissetofprocedureswassubmittedby
3 3
Lou Messerle and Rinaldo Poli. Chapter 2 covers the synthesis of a number of
cyclopentadienyl compounds, including a novel route to sodium and potassium
cyclopentadienide,MC H .SpecialthanksareduetoJohnBercaw,EndyMin,and
5 5
GedParkinforthesynthesesofthebis(pentamethylcyclopentadienyl)compounds
ofgroups3,4,5,and6.Chapter3detailssyntheticproceduresforarangeofmetal–
metal bonded compounds, including several with metal–metal multiple bonds.
Special thanks here are due to Al Cotton, Carlos Murillo, and Dick Walton.
Chapter 4 contains procedures for a range of early and late transition metal
compounds, each a useful synthon for further synthetic elaboration. Chapter 5
dealswiththesynthesisofanumberofmaingroupcompoundsandligands,while
Chapter 6 covers teaching laboratory experiments. The editors are grateful to
Marcetta Darensbourg for suggesting the teaching chapter.
WewouldliketothankeveryonewhosubmittedsynthesesforVolume36and
the checkers who dedicated considerable time and effort in checking the proce-
dures.Weacknowledgethelongdelayingettingthisvolumepublishedandthank
thecontributorsandcheckersfortheirpatience.Tothosecontributorswhowillnot
see their syntheses in this volume, we apologize for not being able to find an
individual willing or able to check their syntheses. We wish to extend special
thanks to Vera Mainz for her expert help in the preparation of the cumulative
indicesthatappearattheendofthisvolume. Weundertookthislargeprojectinthe
hope that readers will find this material to be useful aids to locating recipes that
have appeared since the last cumulative index, which summarized content up
through volume 30 of Inorganic Syntheses.
v
vi Preface
Finally,wewouldliketothankourfriendandcolleagueTomRauchfussforhis
tireless encouragement and advice, and our mentors Dick Andersen and Geoff
Wilkinson(forGSG)andWardSchaapandJohnFackler(forAPS)whotaughtus
both the joys and challenges of synthetic inorganic chemistry.
ALFRED P. SATTELBERGER
ArgonneNationalLaboratory
GREGORY S. GIROLAMI
UniversityofIllinoisatUrbana-Champaign
DEDICATION
This volume is dedicated to the memory of eight eminent chemists who made
outstanding contributions to inorganic chemistry in general and to Inorganic
Syntheses in particular. We also note the recent passing of two other inorganic
chemists,BillLipscombandGordonStone,whowerenotformervolumeeditors
but whose contributions to inorganic chemistry were significant. Each was a
talented synthetic chemist in his own right, and all helped shape the discipline
we know and love.
GEORGETHERALDMOELLER(EDITOR-IN-CHIEF,
VOLUMEV,1957)
TheraldMoellerwasborninNorthBend,Oregon,onApril3,1913,anddiedin
BrokenArrow,Oklahoma,onNovember 24,1997,attheageof84.In1934,he
graduatedfromOregonStateCollege(nowOregonStateUniversity)inCorvallis
asthetopstudentofhisseniorclass,havingmajoredinchemicalengineering.In
1938,hereceivedhisPh.D.degreeininorganicandphysicalchemistryfromthe
UniversityofWisconsin,Madison,forathesistitled“AStudyofthePreparation
andCertainPropertiesofHydrousLanthanumOxideSols,”carriedoutunderthe
direction of Francis C. Krauskopf. Therald was Instructor in Chemistry at
Michigan State College (now Michigan State University) at East Lansing
(1938–1940), but in 1940 he moved to the University of Illinois, Urbana-
Champaign. In 1969, Therald became Chair of the Department of Chemistry at
ArizonaStateUniversityinTempe,servinginthiscapacityuntil1975.Heretired
as Professor Emeritus in 1983.
Theraldbecameaninternationallyrecognizedauthorityonthechemistryofthe
rare earth elements (lanthanides) and published 94 research papers and books in
this area alone. During his 45 years of teaching and research, he guided the
laboratoryresearchof43Ph.D.students,20postdoctoralfellows,and11M.S.and
25B.S.studentsforatotalof99researchstudentsininorganicchemistry.Ofthese,
at least 39 became professors themselves at universities in the United States,
Taiwan, Spain, India, Japan, Brazil, England, and Finland. Several became
Department Chairs and one a College President.
Therald’s281publicationsinclude22booksandlaboratorymanualsauthored
or edited by him (32 books if Spanish, Russian, Japanese, Italian, and Polish
editionsarecounted).Oneofthesetexts,InorganicChemistry,AnAdvancedText
(Wiley, 1952), was the “bible” of inorganic chemistry for decades, enjoying
vii