K. Kasai and M. Fujita
were unique (Rint =0.0638), 4189 observed reflections (I>2s(I)), 369 pa-
rameters, final R1 =0.1436, wR2 =0.3028.
Acknowledgments
We thank Dr. Masaru Aoyagi and Dr. Kumar Biradha for performing the
single-crystal X-ray diffraction studies.
X-ray structural data for 11 f: C58H40Br2CdF12N6O7, Mr =1433.18, ortho-
rhombic, space group Pnnn, a=13.3884(16), b=15.8530(19), c=
26.729(3) , V=5673.0(12) 3, T=153 K, Z=4, 1calcd =1.678 gcmÀ3
,
2qmax =28.048, m
(MoKa)=1.892 mmÀ1, 36143 reflections were collected of
G
which 6875 were unique (Rint =0.0404), 4357 observed reflections (I>
2s(I)), 386 parameters, final R1 =0.0573, wR2 =0.1758.
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X-ray structural data for 11g: C62H44CdF12N6O6, Mr =1309.43, ortho-
rhombic, space group Pnnn, a=13.494(5), b=15.664(5), c=26.830(5) ,
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were unique (Rint =0.0478), 3837 observed reflections (I>2s(I)), 443 pa-
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X-ray structural data for 12: C73H47Cd2F18N11O13, Mr =1853.02, monoclin-
ic, space group P21/n, a=8.864(5), b=28.744(5), c=13.854(5) , b=
90.858(5)8, V=3529(2) 3, T=153 K, Z=2, 1calcd =1.744 gcmÀ3, 2qmax
=
28.028, m
(MoKa)=0.725 mmÀ1, 22329 reflections were collected of which
G
8160 were unique (Rint =0.0279), 5850 observed reflections (I>2s(I)),
550 parameters, final R1 =0.0549, wR2 =0.1473.
X-ray structural data for 13: C64H56CdF12N6O12, Mr =1441.55, monoclinic,
space group C2/c, a=31.552(5), b=13.533(2), c=17.318(3) , b=
121.816(2)8, V=6283.8(17) 3, T=173 K, Z=4, 1calcd =1.524gcm À3
,
2qmax =28.118, m
(MoKa)=0.450 mmÀ1, 19868 reflections were collected of
G
which 7359 were unique (Rint =0.0249), 5828 observed reflections (I>
2s(I)), 448 parameters, final R1 =0.0386, wR2 =0.1002.
X-ray structural data for 14a: C60H44CdF12N6O6, Mr =1285.41, monoclin-
ic, space group P21/c, a=8.1700(13), b=20.445(3), c=16.354(3) , b=
100.204(3)8, V=2688.6(7) 3, T=153 K, Z=2, 1calcd =1.588 gcmÀ3
,
2qmax =27.908, m
(MoKa)=0.508 mmÀ1, 17157 reflections were collected of
A
which 6273 were unique (Rint =0.0273), 4662 observed reflections (I>
2s(I)), 449 parameters, final R1 =0.0271, wR2 =0.0604.
X-ray structural data for 14b: C120H80Cd2F24N12O20, Mr =2690.76, mono-
clinic, space group Cc, a=16.286(2), b=40.817(5), c=16.875(2) , b=
99.467(2)8, V=11065(2) 3, T=153 K, Z=4, 1calcd =1.615 gcmÀ3, 2qmax
=
27.998, m
(MoKa)=0.503 mmÀ1, 30648 reflections were collected of which
A
19523 were unique (Rint =0.0239), 13543 observed reflections (I>2s(I)),
1604parameters, final R1 =0.0402, wR2 =0.0843.
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CCDC-282132 (1a), -282126 (1b), -282130 (2a), -282128 (2b), -282131
(2c), -282125 (2d), -282127 (3), -282129 (4), -282133 (5a), -282134( 5b),
-282140 (6a), -282141 (6b), -282138 (6c), -282142 (6d), -282137 (6e),
-282143 (6 f), -282144 (6g), -282135 (6h), -282150 (7), -282147 (8a),
-282149 (8b), -282148 (8c), -282146 (8d), -282145 (8e), -282159 (9),
-282158 (10a), -282161 (10b), -282157 (10c), -282164( 11a), -282162
(11b), -282163 (11c), -282160 (11d), -282156 (11e), -282155 (11 f),
-282171 (11g), -282170 (12), -282167 (13), -282166 (14a), and -282169
(14b) contain the supplementary crystallographic data for this paper.
These data can be obtained free of charge from the Cambridge Crystallo-
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Attempts to obtain clathrate networks from bpb: The reaction of Cd-
A
0.06 mmol) in ethanol (1 mL), and phenyl acetate (0.24mL, 1.9 mmol)
was attempted under the same reaction conditions as for bpf. After the
mixture was allowed to stand for 48 h at room temperature, [Cd
A
ACHTREUNG
(6.1 mg). The structure was identified by preliminary X-ray measurement
of a single crystal to determine the unit cell parameters and space group.
Elemental analysis calcd (%) for C27H24CdN5O6 ([Cd
N
N
51.73, H 3.86, N 11.17; found: C 51.71, H 3.20, N 11.05. The same reac-
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tion in the presence of N,N-dimethylaniline or m-xylene also gave [Cd-
A
N
These structures were identified by preliminary X-ray measurements of
single crystals.
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