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Inorganic Chemistry in Focus III

Edited by
Gerd Meyer, Dieter Naumann and Lars Wesemann
Inorganic Chemistry
in Focus III

Edited by
Gerd Meyer,
Dieter Naumann
and Lars Wesemann
Related Titles

Meyer, G., Naumann, D., Wesemann, L. (Eds.)

Inorganic Chemistry Highlights

2002, ISBN 3-527-30265-4

Meyer, G., Naumann, D., Wesemann, L. (Eds.)

Inorganic Chemistry in Focus II

2005, ISBN 3-527-30811-3

Driess, M., Nöth, H. (Eds.)

Molecular Clusters of the Main Group Elements

2004, ISBN 3-527-30654-4

Balzani, V. (Ed.)

Electron Transfer in Chemistry

5 Volumes
2001, ISBN 3-527-29912-2
Inorganic Chemistry in Focus III

Edited by
Gerd Meyer, Dieter Naumann and Lars Wesemann
The Editors n All books published by Wiley-VCH are carefully
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Universität zu Köln errors. Readers are advised to keep in mind that
Greinstr. 6 statements, data, illustrations, procedural details or
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Prof. Dr. Dieter Naumann

Institut für Anorganische Chemie
Universität zu Köln
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A catalogue record for this book is available
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Dedicated to Professor John D. Corbett on the occasion of his 80th birthday
 VII

In Praise of Synthesis
This book is about passion. A passion for chemistry. A passion for John D. Cor-
bett, Distinguished Professor of Science and Humanities at Iowa State Univer-
sity of Science and Technology and Senior Chemist at the Ames Laboratory. A
passion and admiration for John’s way of conducting research in solid state
chemistry and for the way he passes on his vast amount of accumulated knowl-
edge to his students, postdoctoral associates and the community as a whole.
John Corbett is a truly outstanding solid state inorganic chemist, an individual
of immense and different talents, who has influenced not only his discipline
but, in many ways, has led the renaissance in solid state chemistry over the past
several decades.
“First comes the synthesis.” What else? But it is as simple as that. It must
have been sheer luck, both for him and for the scientific community, or per-
haps, fate, that John D. Corbett, born in Yakima, Washington, on March 23rd,
1926, with a Ph.D. in physical chemistry (!) from the University of Washington,
received a joint appointment in 1952 as Assistant Professor at the Department
of Chemistry and as Associate Chemist at the Ames Laboratory of the Atomic
Energy Commission (now the U.S. Department of Energy), founded and guided
by the late Frank H. Spedding. It is no wonder that, after some 50 years, John
D. Corbett was the recipient of the 11th Frank H. Spedding Award. This honour
came late, after many others, of which his election to the National Academy of
Sciences (1992) and the ACS Awards in Inorganic Chemistry (1986) and for
Distinguished Service in the Advancement of Inorganic Chemistry (2000), are
three other prominent examples.
But first the “synthesis” had to come! John was interested in reduced metal
halides, particularly for the post-transition metals cadmium, gallium, and bis-
muth (his Ph.D. dissertation was on anhydrous aluminum halides and mixed
halide intermediates, a good start for what was to come!). However, he was not
yet actively interested in rare-earth metals and their remarkable solubility in
their halides. But these elements lured him one floor below where Adrian
Daane headed the metallurgy section of Spedding’s empire. He knew how to
produce rare-earth metals with high purity and in sufficient quantity and also
how to handle tantalum containers. What if one “gave it a try” and reduced
some rare-earth metal halides (John insists that this term is used correctly)
from their respective metals at high temperatures under appropriate conditions,
VIII In Praise of Synthesis

in tantalum or niobium containers? This soon gave rise to a whole number of

rare-earth metal subhalides, both metallic and salt-like.
It is surely always difficult to imagine the unimaginable. The “eighth wonder
of the rare-earth world” had yet to be discovered. It was, in fact, discovered in a
tantalum ampoule as the fantastic gadolinium sesquichloride. Clusters became
a passion, they were found everywhere throughout the periodic table, of course
with reduced rare-earth metal halides and their “garbage chemistry”, as Bob
McCarley coined it, in a friendly manner. Zirconium chemistry was an obses-
sion for while, post-transition polyanions and cations, Zintl phases, tellurides,
non-carbon fullerenes and, recently, approximants and quasicrystals. John
beams boyishly when he talks about his and his co-workers latest achievements.
“But there is no time to rest. There is so much which is unimaginable out
there”. “Explore!” “Lord, grant me patience, but hurry.”
John’s contributions to the development of solid state chemistry are particular-
ly noteworthy. Together with industrial and academic chemists interested in this
subject, Corbett and others have encouraged and fostered this important area of
chemistry. Likewise, in the role of teacher and advisor, John Corbett motivates
and encourages young people towards a career in science. His influence on an
entire generation of inorganic and solid state chemists uniquely endears John to
his many friends around the world.
As a writer and author John is also well known for many “Corbett Quotables”,
of which we have already mentioned a few above. Here are a few other endur-
ing examples:
“Exploratory solid state synthesis seems to be the only workable route to new
phases because of a general inability to predict relative phase stabilities and
thence structures or compositions”, published in “K4La6I14Os: A new Structure
Type for Rare-Earth-Metal Cluster Compounds that Contain Discrete Tetrahedral
K4I3+ Units.” S. Uma, J. D. Corbett, Inorg. Chem. 1999, 38, 3831–3835.
“The diverse instances in which efficient, space-filling, bonding arrangements
repeat is both surprising and pleasing”, published in “Synthesis, Structure, and
Bonding of BaTl3: An Unusual Competition between Cluster and Classical
Bonding in the Thallium Layers.” D.-K. Seo, J. D. Corbett, J. Am. Chem. Soc.
2002, 124, 415–420.
“The best discoveries in an unprincipled area are often those that one stum-
bles upon during experiments designed with plausible but incorrect or naïve
ideas regarding possible compounds or structural targets”, published in “Diverse
Solid-State Clusters with Strong Metal–Metal Bonding. In Praise of Synthesis.”
J. D. Corbett, J. Chem. Soc., Dalton Trans. 1996, 575–587.
“There is much to be discovered that cannot be imagined. It is the wonder
and excitement of finding the unprecedented and unimaginable that makes re-
search enjoyable, even exhilarating, and worthwhile.” Published in “Exploratory
Synthesis in the Solid State. Endless Wonders.” J. D. Corbett, Inorg. Chem. 2000,
39, 5178–591.
Needless to say, John’s energy and enthusiasm for chemistry have not dimin-
ished over 50-plus years of active research but, on the contrary, appear to be on
 In Praise of Synthesis IX

the increase. His recent discoveries of large Buckyball networks of indium, his
election to the National Academy of Sciences, and his Department of Energy’s
Division of Basic Energy Sciences Award for Sustained Outstanding Research,
all attest to his achievements. We wish John a very happy birthday and look for-
ward to many more “Corbett Quotables” in the years to come.

Evanston, IL, and Cologne Kenneth R. Poeppelmeier & Gerd Meyer

Summer 2006
 XI

Contents

Dedicated V

In Praise of Synthesis VII

Preface XIX

List of Contributors XXI

Biographical Sketches XXV

1 Inter-electron Repulsion and Irregularities in the Chemistry

of Transition Series 1
David A. Johnson
1.1 Introduction: Irregularities in Lanthanide Chemistry 1
1.2 A General Principle of Lanthanide Chemistry 4
1.3 Extensions of the First Part of the Principle 6
1.4 Extensions of the Second Part of the Principle 8
1.5 The Tetrad Effect 9
1.6 The Diad Effect 11
References 13

2 Stereochemical Activity of Lone Pairs in Heavier Main-group Element

Compounds 15
Anja-Verena Mudring
2.1 Introduction 15
2.2 When Does a Lone Pair of Electrons Become Stereochemically
Active? – Observations 16
2.3 Theoretical Concepts 17
2.3.1 Molecular/Complex Compounds 18
2.3.2 Solid Materials 20
2.4 Conclusions 25
Acknowledgments 26
References 26
XII Contents

3 How Close to Close Packing? 29

Hideo Imoto
3.1 Introduction 29
3.2 Essential Features of Close Packing 30
3.3 Parameter Definitions 30
3.4 Correlation Between D and N 33
3.5 Transformation of Close-packing Arrangements 35
3.6 Close-packing of Cations or of Anions? 38
3.7 What Determines the Structure? 41
Appendix. ICSD Codes, D and N Parameters of the Structures
Used 42
References 44

4 Forty-five Years of Praseodymium Di-iodide, PrI2 45

Gerd Meyer and Andriy Palasyuk
Foreword 45
4.1 Introduction 46
4.2 Phases and Structures in the System Praseodymium-Iodine 47
4.2.1 Synthesis Generalities 47
4.2.2 Structural Principles 48
4.3 PrI2: Phases and Phase Analysis 51
4.4 Conclusions 58
Acknowledgments 59
References 59

5 Centered Zirconium Clusters: Mixed-halide Systems 61

Martin Köckerling
Foreword 61
5.1 The Basics of Zirconium Cluster Chemistry 61
5.2 Motivation 62
5.3 Mixed-Chloride-Iodide Zirconium Cluster Phases
with a 6 : 12–Metal : Halide Ratio 63
5.4 Mixed Chloride–Iodide Zirconium Cluster Phases
with a 6 : 13 Metal : Halide Ratio 64
5.5 Mixed Chloride–Iodide Zirconium Cluster Phases
with a 6 : 14 Metal : Halide Ratio 67
5.6 Mixed Chloride–Iodide Zirconium Cluster Phases
with a 6 : 15 Metal : Halide Ratio 71
5.7 Mixed Chloride–Iodide Zirconium Cluster Phases
with a 6 : 18 Metal : Halide Ratio –
Products from Solid-state Reactions 76
5.8 Outlook 77
Acknowledgments 77
References 77
 Contents XIII

6 Titanium Niobium Oxychlorides: Ligand Combination Strategy

for the Preparation of Low-dimensional Metal Cluster Materials 79
Ekaterina V. Anokhina and Abdessadek Lachgar
Abstract 79
6.1 Introduction 79
6.1.1 Cluster Connectivity and Framework Dimension 81
6.1.2 The Ligand Combination Approach to Creating Anisotropic
Frameworks 82
6.2 Overview of the Chemistry of Niobium Chloride
and Niobium Oxide Cluster Compounds 83
6.2.1 Synthesis and Chemical Properties 83
6.2.2 Electronic Structure, Redox and Magnetic Properties 84
6.3 Niobium Oxychloride Cluster Compounds 85
6.3.1 One-dimensional Cluster Frameworks 85
6.3.1.1 Frameworks Built from Clusters with Five Oxygen Ligands 85
6.3.1.2 Frameworks Built of Clusters with Six Oxygen Ligands 86
6.3.2 Two-dimensional Cluster Frameworks 88
6.3.2.1 2D Oxychloride Frameworks with a Honeycomb-like Structure 88
6.3.2.2 Pillared 2D Oxychloride Frameworks 90
6.3.2.3 2D Framework with Graphite-like Cluster Connectivity 90
6.4 Summary of Crystallographic Data on Titanium Niobium
Oxychlorides 93
6.4.1 Effect of the Total Number of Ligands 93
6.4.2 Cluster Configuration 95
6.4.2.1 Relationships Between Ligand Arrangement and Direct Inter-cluster
Linkages 95
6.4.2.2 Relationships Between the Ligand Arrangement and Inter-cluster
Linkages via Counter-ions 96
6.4.3 Anion Segregation 97
6.4.4 Structure-determining Factors in the Absence of “Hard” Cations 97
6.5 Electronic Configuration of Niobium Oxychloride Clusters 99
6.6 Conclusion and Outlook 100
References 101

7 Trinuclear Molybdenum and Tungsten Cluster Chalcogenides:

From Solid State to Molecular Materials 105
Rosa Llusar and Cristian Vicent
7.1 Introduction 105
7.2 Synthesis and Structure of Molecular M3Q4 and M3Q7 Cluster
Complexes 107
7.2.1 Solid-state Synthesis: Dimensional Reduction 108
7.2.2 Solution Routes: Excision 109
7.2.3 Ligand Exchange Reactions 112
7.2.3.1 M3Q4 Cluster Complexes 112
7.2.3.2 M3Q7 Cluster Complexes 113
XIV Contents

7.3 Trinuclear Clusters as Building Units 115

7.3.1 Molecular Conductors Based on M3Q7 Cluster Complexes 115
7.3.2 Formation of Supramolecular Adducts 117
Acknowledgments 119
References 119

8 Current State on (B,C,N) Compounds of Calcium

and Lanthanum 121
H.-Jürgen Meyer
8.1 Introduction 121
8.2 Problems and Pitfalls of some Calcium Compounds with (mixed)
B,C,N Anions 121
8.2.1 Borides of Calcium and Lanthanum 123
8.2.2 The CaC2 Problem and Ca3Cl2C3 124
8.2.3 Calcium Nitride and Calcium Carbodiimides 126
8.2.4 Calcium Nitridoborates 126
8.2.5 A Comparison of Ca3(BN2)2 and Sr3(BN2)2 Structures 126
8.3 Metal-nitridoborates 129
8.3.1 Electronic Considerations 129
8.4 Lanthanum Nitridoborates 131
Compounds in Ca-B-N and La-B-N systems 132
8.4.1 Nitridoborate Ions 133
8.4.2 Structures of Lanthanum Nitridoborates 134
8.5 Outlook 137
Acknowledgments 138
References 138

9 Compositional, Structural and Bonding Variations in Ternary Phases

of Lithium with Main-group and Late-transition Elements 141
Claude H. Belin, Monique Tillard
9.1 Introduction 141
9.2 Tuning Structures and Properties in Lithium Binary and Ternary
Systems 142
9.3 Clustering in Condensed Lithium Ternary Phases: A Way Towards
Quasicrystals 143
9.4 Exploration of New Lithium Ternary Systems Containing Ag, Zn, Al,
Si, Ge 144
9.4.1 Background 144
9.4.2 The System Li-Al-Ag 145
9.4.3 Compositional and Structural Variations in the System Li-Al-Si 146
9.4.4 The Tetragonal Compound Li9AlSi3, a Good Anodic Material 148
9.5 The Intermetallic Li-Zn-Ge System, from Electron-poor
to Electron-rich Phases 149
9.5.1 The Electron-poor Hexagonal Phase LiZnGe 149
9.5.2 The True Cubic Configuration of the Compound Li2ZnGe 150
 Contents XV

9.5.3 The Li-rich Compound Li8Zn2Ge3 with an Open-layered Anionic

Framework 152
9.6 Concluding Remarks 154
References 154

10 Polar Intermetallics and Zintl Phases along the Zintl Border 157
Arnold M. Guloy
10.1 “First comes the synthesis . . .” – J. D. Corbett 157
10.2 What are Intermetallics? 157
10.3 The Zintl-Klemm Concept 160
10.4 “Electron-poor” Polar Intermetallics 161
10.5 Intermetallic p-Systems 162
10.6 Some Final Remarks 168
References 169

11 Rare-earth Zintl Phases:

Novel Magnetic and Electronic Properties 173
Susan M. Kauzlarich and Jiong Jiang
11.1 Introduction 173
11.2 Structure 174
11.3 Resistivity 177
11.4 Magnetic Properties 178
11.5 Magnetoresistance 179
11.6 Summary 180
Acknowledgments 181
References 181

12 Understanding Structure-forming Factors

and Theory-guided Exploration of Structure–Property Relationships
in Intermetallics 183
Dong-Kyun Seo, Li-Ming Wu and Sang-Hwan Kim
12.1 Introduction 183
12.2 Mn14Al56+xGe3-x (x = 0.00, 0.32, 0.61) 184
12.3 La5-xCaxGe4 (x = 3.37, 3.66, 3.82) and Ce5-xCaxGe4
(x = 3.00, 3.20, 3.26) 188
12.4 Concluding Remarks 191
Acknowledgments 191
References 192

13 Ternary and Quaternary Niobium Arsenide Zintl Phases 195

Franck Gascoin and Slavi C. Sevov
13.1 Introduction 195
13.2 New Main-group Arsenides 197
13.3 Compounds Based on Isolated [NbAs4] Tetrahedral Centers 199
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