Crystal Engineering Using Bis- and Tris-phenols. Adducts with 1,4,8,11-Tetraazacyclotetradecane (Cyclam): Isolated Ladders in the Adduct with 4,4'-Thiodiphenol, Tethered Ladders in the Adduct with 4,4'-Sulfonyldiphenol and Two Interwoven Three-Dimensional Networks in the Adduct with 1,1,1-Tris(4-hyd
Crystal Engineering Using Bis- and Tris-phenols. Adducts with 1,4,8,11-Tetraazacyclotetradecane (Cyclam): Isolated Ladders in the Adduct with 4,4'-Thiodiphenol, Tethered Ladders in the Adduct with 4,4'-Sulfonyldiphenol and Two Interwoven Three-Dimensional Networks in the Adduct with 1,1,1-Tris(4-hyd
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使用双酚和三酚的晶体工程。
DOI：
10.1107/s0108768197010136
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发表时间：
1998
期刊：
影响因子：
--
通讯作者：
P. R. Meehan
中科院分区：
文献类型：
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作者：
G. Ferguson;C. Glidewell;Richard M. Gregson;P. R. Meehan
4，4 ′-硫代二酚-1，4，8，11-四氮杂环十四烷（21）的结构，（C12 H10 O2 S）2.C10H24N4（1），单斜晶系，P21/c，a = 11.1602（12），B = 10.8084（12），c = 14.001（2）A，β = 103.127（10）°，Z = 2，含有酚盐阴离子[HOC 6 H4 SC 6 H4 O]−和双质子化环拉胺阳离子[C10 H26 N4]2+：这些阳离子具有中心对称的反式-III构象，并且两个额外的质子包含在大环的N4空腔内，由三中心氢键保持。 酚盐阴离子形成链，通过O-H-O氢键结合在一起，这些链对通过[cyclam H2]2+阳离子通过N-H-O氢键交联成梯形。4，4 '-磺酰基双酚-1，4，8，11-四氮杂环十四烷（2/1）的结构，（C12 H10 O 4S）2.C10H24N4（2），三斜晶系，P1 ′，a = 10.9345（10），B = 11.0060（10），c = 14.350（2）A，α = 79.532（10），β = 86.739（10），γ = 87.471（10）°，Z = 2，含有酚盐阴离子[HOC 6 H4 SO2 C6 H4 O]−和环拉胺二价阳离子[C10 H26 N4]2+：酚盐阴离子连接成反平行链，由环拉胺阳离子交联。 在结构中有两种不同类型的梯子，分别沿沿着（0，y，0）和（1\over2，y，1\over2）延伸，并且这些捆绑的梯子通过C-H-O氢键连接在一起以形成连续的三维阵列。在1，1，1-三（4-羟基苯基）乙烷-1，4，8，11-四氮杂环十四烷-甲醇（2/1/1），（C20 H18 O3）2.C10H24N4.CH4O（3），三斜晶系，P1 ′，a = 8.2208（11），B = 16.245（2），c = 17.337（2）A，α = 81.694（13），β = 89.656（14），γ = 86.468（12）°，Z = 2，该结构包含与（1）中发现的类型完全相同的中心对称双质子化cyclam阳离子，酚盐阴离子[（HOC 6 H4）2C（CH 3）C6 H4 O]−和中性甲醇分子。 分子组分通过九种不同类型的氢键连接在一起，其中五种为O-H O型，四种为N-H O型，形成沿[001]、[010]（两组）、[211]和[211 ']方向延伸的链。这些链图案的组合产生两个独立的三维网络，它们完全交织在一起，但彼此不结合。
The structure of 4,4′-thiodiphenol–1,4,8,11-tetraazacyclotetradecane (2/1), (C12H10O2S)2.C10H24N4 (1), monoclinic, P21/c, a = 11.1602 (12), b = 10.8084 (12), c = 14.001 (2) A, β = 103.127 (10)°, with Z = 2, contains phenolate anions [HOC6H4SC6H4O]− and diprotonated cyclam cations [C10H26N4]2+: these cations have the centrosymmetric trans-III conformation and the two additional protons are contained within the N4 cavity of the macrocycle, held by three-centre hydrogen bonds. The phenolate anions form chains, held together by O—H⋯O hydrogen bonds, and pairs of these chains are cross-linked into ladders by the [cyclamH2]2+ cations by means of N—H⋯O hydrogen bonds. The structure of 4,4′-sulfonyldiphenol–1,4,8,11-tetraazacyclotetradecane (2/1), (C12H10O4S)2.C10H24N4 (2), triclinic, P1¯, a = 10.9345 (10), b = 11.0060 (10), c = 14.350 (2) A, α = 79.532 (10), β = 86.739 (10), γ = 87.471 (10)°, with Z = 2, contains phenolate anions [HOC6H4SO2C6H4O]− and cyclam dications [C10H26N4]2+: the phenolate anions are linked into antiparallel chains, cross-linked by the cyclam cations. There are two distinct types of ladder in the structure running along (0, y, 0) and (1\over2, y, 1\over2), respectively, and these bundled ladders are tied together by C—H⋯O hydrogen bonds to form a continuous three-dimensional array. In 1,1,1-tris(4-hydroxyphenyl)ethane–1,4,8,11-tetraazacyclotetradecane–methanol (2/1/1), (C20H18O3)2.C10H24N4.CH4O (3), triclinic, P1¯, a = 8.2208 (11), b = 16.245 (2), c = 17.337 (2) A, α = 81.694 (13), β = 89.656 (14), γ = 86.468 (12)°, with Z = 2, the structure contains centrosymmetric diprotonated cyclam cations of precisely the same type as found in (1), phenolate anions [(HOC6H4)2C(CH3)C6H4O]− and neutral methanol molecules. The molecular components are linked together by nine different types of hydrogen bond, five of O—H⋯O type and four of N—H⋯O type, to form chains running in the [001], [010] (two sets), [211] and [211¯] directions. The combination of these chain motifs generates two independent three-dimensional networks which are fully interwoven, but not bonded to one another.