greater general demand for crystal structures, fuelled the technological development
of instrumentation capable of providing a higher throughput, but still relied on
manual operation. This phase of technical progression powered significant developments in the 1960s and 1970s which saw the birth of ‘chemical crystallography’ as a
distinct subject area. At the time, the main driver in chemical crystallography was the
demand to establish the identity of synthesised compounds, and perhaps the most
significant contribution to this came from a burgeoning organometallic chemistry
community that had a need to characterise structural features and bonding in the vast
number of exciting new compounds they produced. At this time, a crystallography
laboratory would produce about one structure a month (about 500 reflections could
be measured in a working day, and hence the size of the structure also had a big
influence on data collection time). During the 1970s, instrumentation moved away
from manual operation and became increasingly computer-automated, and, also,
access to computing facilities and software for structure refinement became more
available. The laboratory throughput rose to around 2–3 structures per week. During
the 1980s, in-house mainframe computing became accessible, generating another
increase in throughput and the transition to a service culture – however, the output of
the laboratory essentially depended on how many diffractometers were available!
The 1990s saw the (re)introduction of area detection methods and low-cost personal
computing, and by the middle of this decade, charge-coupled device (CCD) detectors prevailed. These instruments could readily produce two datasets in a 24-h
period. Also at this time, synchrotron-based instrumentation became available for
chemical crystallography [2]. These facilities were still largely based on traditional
laboratory equipment, but they provided the ability to look at smaller and more
weakly diffracting crystals – this considerably expanded the range of science
addressable by the technique.
Chemical crystallography became a thriving discipline as a result of these innovations. For example, the notion of crystal engineering was born and quickly
grasped by a range of communities going far beyond the realm of the individual
crystallography group. Crystal engineers are not the only example of the adoption of
chemical crystallography by modern chemistry fields – the rapid growth of supramolecular chemistry and metal-organic framework design has been based in part on
the revealing nature of crystal structure results. Furthermore the service crystallography culture has also become thoroughly embedded as a popular tool for the
synthetic chemist, in part due to the unambiguous nature of a crystal structure result,
but also to the fact that in many cases the ‘waiting time’ to get a result has become
comparable to that of commonly used spectroscopic methods.
Additionally, these advances in instrumentation have fuelled the rise of more
advanced single-crystal techniques in chemistry, such as high pressure [3, 4], in situ
process monitoring [5] and photocrystallography-based studies [6]. This review is
concerned primarily with service crystallography, but it will touch on some of the
implications that advances in this area have for these techniques.
This review begins by considering the notion of the modern ‘chemical crystallography facility’. That is, driven by the nature and volume of samples examined, the
practice of service chemical crystallography now generally needs to go beyond
Leading Edge Chemical Crystallography Service Provision and Its Impact on. . .
71
of instrumentation capable of providing a higher throughput, but still relied on
manual operation. This phase of technical progression powered significant developments in the 1960s and 1970s which saw the birth of ‘chemical crystallography’ as a
distinct subject area. At the time, the main driver in chemical crystallography was the
demand to establish the identity of synthesised compounds, and perhaps the most
significant contribution to this came from a burgeoning organometallic chemistry
community that had a need to characterise structural features and bonding in the vast
number of exciting new compounds they produced. At this time, a crystallography
laboratory would produce about one structure a month (about 500 reflections could
be measured in a working day, and hence the size of the structure also had a big
influence on data collection time). During the 1970s, instrumentation moved away
from manual operation and became increasingly computer-automated, and, also,
access to computing facilities and software for structure refinement became more
available. The laboratory throughput rose to around 2–3 structures per week. During
the 1980s, in-house mainframe computing became accessible, generating another
increase in throughput and the transition to a service culture – however, the output of
the laboratory essentially depended on how many diffractometers were available!
The 1990s saw the (re)introduction of area detection methods and low-cost personal
computing, and by the middle of this decade, charge-coupled device (CCD) detectors prevailed. These instruments could readily produce two datasets in a 24-h
period. Also at this time, synchrotron-based instrumentation became available for
chemical crystallography [2]. These facilities were still largely based on traditional
laboratory equipment, but they provided the ability to look at smaller and more
weakly diffracting crystals – this considerably expanded the range of science
addressable by the technique.
Chemical crystallography became a thriving discipline as a result of these innovations. For example, the notion of crystal engineering was born and quickly
grasped by a range of communities going far beyond the realm of the individual
crystallography group. Crystal engineers are not the only example of the adoption of
chemical crystallography by modern chemistry fields – the rapid growth of supramolecular chemistry and metal-organic framework design has been based in part on
the revealing nature of crystal structure results. Furthermore the service crystallography culture has also become thoroughly embedded as a popular tool for the
synthetic chemist, in part due to the unambiguous nature of a crystal structure result,
but also to the fact that in many cases the ‘waiting time’ to get a result has become
comparable to that of commonly used spectroscopic methods.
Additionally, these advances in instrumentation have fuelled the rise of more
advanced single-crystal techniques in chemistry, such as high pressure [3, 4], in situ
process monitoring [5] and photocrystallography-based studies [6]. This review is
concerned primarily with service crystallography, but it will touch on some of the
implications that advances in this area have for these techniques.
This review begins by considering the notion of the modern ‘chemical crystallography facility’. That is, driven by the nature and volume of samples examined, the
practice of service chemical crystallography now generally needs to go beyond
Leading Edge Chemical Crystallography Service Provision and Its Impact on. . .
71