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Elemental Analysis: calcd for C

2·H

O) C 55.30 % H 4.18 %, found C 55.49 % H

3.91 %

2.5 [Zn

(L1)(H

]·2H

O (1)

Zn(ClO

)

·6H

O (0.112 g, 0.30 mmol) and butane tetraacid H

L2 (0.042 g, 0.10 mmol) were

added to a Parr 23 ml pressure vessel with Teflon liner followed by DMF (3 ml), ethanol (3 ml)

and distilled water (2 ml). The flask was sealed and heated at 95 ºC for 48 hours before being

cooled down to room temperature at 0.1 ºC min

-1

. The colourless crystalline product was

collected by filtration and included crystals suitable for single crystal diffraction study. Yield

0.039 g (59.7 %). Elemental analysis: calcd for Zn

C 36.78 % H 4.01 %; found C

36.72 % H 3.74 %.

2.6 [Zn

(L2)

(DMF)

]·4H

O (2)

Zn(ClO

)

·6H

O (0.112 g, 0.30 mmol) and butene tetraacid H

L1 (0.042 g, 0.10 mmol) were

added to a Parr 23 ml pressure vessel with Teflon liner followed by DMF (3 ml), ethanol (3 ml)

and distilled water (2 ml). The flask was sealed and heated at 95 ºC for 48 hours before being

cooled down to room temperature at 0.1 ºC min

-1

. The colourless crystalline product was

collected by filtration and included crystals suitable for single crystal diffraction study. Yield

0.051 g (35.6 %). Elemental analysis: calcd for Zn

C 41.11 % H 4.15 % N 2.94 %;

found C 40.64 % H 3.95 % N 2.56 %. The powder diffraction pattern of the bulk sample was

consistent with that calculated from the single crystal diffraction data.

3. Crystallography

3.1 Single Crystal Diffraction

Crystals of 1 and 2 were mounted using a viscous hydrocarbon oil to coat the crystal on a thin

carbon fibre attached to the end of a borosilicate glass capillary. X-ray data were collected on

synchrotron beam line 16.2smx at the Synchrotron Radiation Source at the CCLRC Daresbury

Laboratory at 100 K. For each compound, data were corrected for absorption using empirical

methods (SADABS) based upon symmetry equivalent reflections combined with measurements

at different azimuthal angles [1]. Crystal structures were solved and refined against all F

values

using the SHELXTL suite of programs [2]. Non-hydrogen atoms were refined anisotropically

(when no disorder was present) and hydrogen atoms associated with oxygen atoms were located

from the difference map and the O–H distance fixed at 0.96 Å. All other hydrogen atoms were

placed in calculated positions with idealised geometries and refined using a riding model. In 2,

three of the four uncoordinated water molecules have the oxygen atom disordered over two sites

and have been modelled with 59(1):41(1), 72(2):28(2) and 58(2):42(2) ratios respectively.

Hydrogen atoms were not modelled on the disordered water molecules. Views of the two-fold

interpenetrated diamondoid network adopted by 2 are shown in Figures S1 and S2.

Table S1. Data collection, Structure Solution and Refinement Parameters for 1 and 2

1 2

Crystal colour Colourless Colourless

Formula Zn

326.57 1431.67

Crystal size (mm) 0.06 x 0.06 x 0.06 0.20 x 0.13 x 0.03

Crystal system Triclinic Triclinic

Space group, Z P-1, 1 P-1, 2

a (Å) 7.6916(15) 13.0757(6)

1 2 3 4 5 6 7 8 9 10 11

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