Institute of organic chemistry National academy of sciences of Ukraine

 



     X-RAY MONO-CRYSTAL DIFFRACTOMETRY CENTER

    GENERAL POSITIONS:

    1.1 The Center of joint scientific equipment usage “X-Ray Mono-Crystal Diffractometry” is established on the basis of the Institute of Organic Chemistry of the NASU with the aim of efficient usage of the unique and precious X-Ray mono-crystal diffractometry complex APEX II (“Bruker”, USA/Germany/the Netherlands) (further on - Device).   Scientific research of the Center is directed to the study of molecular and crystalline structure of organic, inorganic and organo-element compounds.

    • 1.2 Institute of Organic Chemistry of the NASU has all the facilities for the Device: a special premises, specialists of international level and experience (investigations on the similar equipment in Great Britain, Canada, Germany, Switzerland).  

     

    • 1.3 The Center “X-Ray Mono-Crystal Diffractometry” assumes overall responsibility for a qualitative continuous work of the Device, its maintenance and efficient usage.

    The Structure, Tasks and Work Schedule of the Center:

    2.1 The Center is a property of the National Academy of Sciences of Ukraine. The Device is on the balance of the Institute of Organic Chemistry of the NASU.

    2.2 The Center is a scientific department of the Institute of Organic Chemistry of the NASU, it is subordinated to the Management of the Institute directly. The Center is named “X-Ray Mono-Crystal Diffractometry” what was affirmed by the Commission on Scientific Equipment Modernization of the Presidium of the NASU (Commission) alongside with the Provisions of the Center.
    2.3 The main aim of the Center is to conduct study on the Device using experienced personnel and to keep the Device in the regime of optimal functioning, to give consultations to the scientists.
    2.4 The Head of the Center is Doctor of Science Chernega O.M., general supervisor is Deputy Director on Science Professor Shermolovich Yu.G.
    2.5 Once per year the Institute gives a report on the Work of the Center to the Bureau of Chemistry Subdivision of the NAS of Ukraine, and in case of the necessity – to the Commission.

    Service Provision Order:

    3.1 Information about the Center is represented at the web-sites of the Institute of Organic Chemistry and Presidium of the NAS of Ukraine.
    3.2 Scientific institutions having the necessity to conduct study on the X-Ray Diffractometer Bruker APEX II should submit an application in  written form to the Bureau of Chemistry Subdivision of the NASU twice a year: before January, 15 and before June, 15, the application should include request for the quantity of hours, terms, types of study.

    • 3.3 The Bureau of Chemistry Subdivision of the NASU affirms the working hours division among the applicants.

     

    • 3.4 Director of the Institute of Organic Chemistry affirms the Work Schedule for the Center by the order coordinated with the Bureau of the Chemistry Subdivision of the NASU.
    • 3.5 Planning the work of the Center, the Director is guided by the proportions pointed in the Direction of the Presidium of the NAS of Ukraine # 322 of 28.04.04.

     

    • 3.6 Working time of the Device is registered in a special diary.
    • 3.7 Chargeable service for the Device usage is given in accordance to the current legislation.

     

    • 3.8 The Institute provides necessary maintenance of the Device at its own expense . In case of repair, its cost is divided between the Clients proportionally to the used working time.

                              Equipment of the Center     
    Mono-Crystal X-Ray Diffractometer SMART APEX II is produced by Bruker Company. The Diffractometer is supplied with a modern two-dimensional CCD detector, shows high sensitivity and speed of information reading. CCD detector of APEX ²² has 1:1 enlargement factor  and scintillator contacts photo-sensitive  CCD chip surface through a thin fiber-optics plate what provides high sensitivity and low level on internal noise, if chip is cooled to  –60°Ñ . Low Temperature attachment of Oxford Cryosystems firm gives an opportunity to conduct experiments at temperatures –190 - +100° Ñ .  
    IMPORTANT !!! The Diffractometer is not assigned for testing of polymer materials, powders and films. The optimal size of mono-crystals acceptable for investigation should be 0.2-0.5 mm to every side. Good quality crystals may be smaller but scanning time in this case is longer. It should be mentioned that the quality, speed of collecting and processing of the data, depend on the quality of the crystal.

    Main Technical Characteristics of the Diffractometer SMART APEX II

    A cermet X-Ray high focus pipe with a molybdenum anode, graphite monochromator, high-speed screens and attenuator are maintained at the diffractometer.    The Device is also equipped with a set of standard collimators 0.3 and 0.5 mm. and a mono-capillary collimator what increases intensity of X-Ray beam.  Goniometer: provides quick data collection of any shape crystals.  Goniometer type – 3-circle. Distance between CCD detector and a sample is 20-320 mm. Detector:  


    CCD chip

    Fairchild 486 4K CCD

    Pixel quantity

    4096 x 4096 (16 Mega-pixels)

    Size of active zone

    62 mm x 62 mm

    Size of CCD pixels

    15m x 15 m

    Enlargement factor

    1:1

    Typical quantum yield

    170 electrons/X-ray photon (Mo)

    Speed of reading

    Quantity of ports-4; to 4 MHz

    Correlation signal-noise for one X-Ray photon  (Mo)

    > 10:1 (SMART 1K detector 0.7:1)


    Low temperature Attachment "Oxford Cryostream 700 Series"

    Active temperature range is 90 - 378 K. Gaseous nitrogen flow 5 or 10 l/min Liquid nitrogen consumption 1-2 l/hour. Maximal speed of temperature change 360 Ê/hour. Precision of temperature support  ±0.1 Ê

     

     

     

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