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首页> 外文期刊>Acta crystallographica. Section C, Structural chemistry. >Synthesis and structural characterization of iridium(I) complexes of 20‐membered macrocyclic rings bearing chelating bis(N‐heterocyclic carbene) ligands
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Synthesis and structural characterization of iridium(I) complexes of 20‐membered macrocyclic rings bearing chelating bis(N‐heterocyclic carbene) ligands

机译：20元大环环轴承螯合双（N-杂环碳烯）配体的铱（I）复合物的合成和结构表征

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摘要

The reactivities of two 20‐membered macrocyclic ligands, each containing two N‐heterocyclic carbene (NHC) and two amine groups, towards [IrCl(COD)] 2 (COD is cycloocta‐1,5‐diene) were investigated. Macrocycles containing imidazolin‐2‐ylidene groups formed the monometallic complex [(1,2,5,6‐η)‐cycloocta‐1,5‐diene](5,16‐dibenzyl‐1,5,9,12,16,20‐hexaazatricyclo[18.2.1.1 9,12 ]tetracosa‐10,21‐dien‐21,22‐diylidene)iridium(I) bromide dichloromethane monosolvate, [Ir(C 8 H 12 )(C 32 H 42 N 6 )]Br·CH 2 Cl 2 , 2a . The structure of iridium complex 2a at 100?K has triclinic P symmetry. The ligand in 2a coordinates to the Ir center through the NHC moieties in a cis fashion. Additionally, the ligand adopts an umbrella‐like structure that appears to envelope the Ir center. The structure displays C—H…Br interactions. Macrocycles containing benzimidazolin‐2‐ylidene groups formed the bimetallic complex [μ‐5,20‐dibenzyl‐1,5,9,16,20,24‐hexaazapentacyclo[22.6.1.1 9,16 .0 10,15 .0 25,30 ]dotriaconta‐10(15),11,13,25(30),26,28‐hexaene‐31,32‐diylidene]bis{bromido[(1,2,5,6‐η)‐cycloocta‐1,5‐diene]iridium(I)}, [Ir 2 Br 2 (C 8 H 12 ) 2 (C 40 H 46 N 6 )], 2b . The structure of complex 2b at 100?K has orthorhombic Pbca symmetry. Each NHC moiety in 2b coordinates in a monodentate fashion to an Ir(COD) fragment. The structure exhibits disorder of the main molecule. This disorder is found in the portion of the macrocycle containing an amine group. This structure also displays C—H…Br interactions. Finally, the structure of the hexafluorophosphate salt of the imidazolin‐2‐ylidene‐containing macrocycle, namely 5,16‐dibenzyl‐1λ 5 ,5,9,12λ 5 ,16,20‐hexaazatricyclo[18.2.1.1 9,12 ]tetracosa‐1(23),10,12(24),21‐tetraene‐1,12‐diium bis(hexafluorophosphate), C 32 H 44 N 6 2+ ·2PF 6 ? , 1c , was determined. The structure of macrocycle 1c at 100?K has triclinic P symmetry and was found to contain C—H…F interactions.
机译：研究了两种20元型大环配体的反应，每种20元致癌配体，各自含有两种N-杂环基石（NHC）和两种胺基，朝向[IRCL（COD）] 2（COD是环胶囊-1,5-二烯）。含有咪唑啉-2- ylidene基团的宏键形成单金属络合物[（1,2,5,6-η）-cycloocta-1,5-二烯]（5,16-二苄基-1,5,9,12,16， 20-六唑氮杂环[18.2.1.19,12] Tetracosa-10,21-DIEN-21,22-二苯基）铱（I）溴化物二氯甲烷单溶化物，[IR（C 8 H 12）（C 32 H 42 N 6）] BR·CH 2 CL 2,2a。铱络合物2a的结构在100〜k下具有三级P p对称性。在2A中的配体通过顺序方式通过NHC部分坐落在IR中心。另外，配体采用类似伞形结构，该结构似乎具有封套IR中心。该结构显示C-H ... BR相互作用。含有Benzimidazolin-2- ylidene基团的宏键形成双金属络合物[μ-5,20-二苄基-1,5,9,16,20,24-六氮杂扎属[22.6.1.19,16 .0 10,15 .0 25， 30] dotriaconta-10（15），11,13,25（30），26,28-六烯-31,32-二亚二苯二甲苯{bromido [（1,2,5,6-η）-cycloocta-1， 5-二烯]铱（I）}，[IR 2 Br 2（C 8 H 12）2（C 40 H 46 N 6）]，2b。络合物2b的结构在100〜k下具有正交的PBCA对称性。在2B中的每个NHC部分以单齿时尚坐标，以IR（COD）片段。该结构表现出主要分子的病症。该疾病存在于含有胺基的宏循环的一部分中。该结构还显示了C-H ... BR互动。最后，含咪唑啉-2-亚基亚甲酰胺的宏循环的六氟磷酸盐的结构，即5,16-二苄基-1λ5,5,9,12λ5,16,20-六己肼（六己肼）[18.2.1.19,12] Tetracosa -1（23），10,12（24），21-四烯-1,12-杜米双（六氟磷酸盐），C 32 H 44 N 6 2+·2PF 6？ ，1C，确定。宏细胞1c的结构在100℃下具有三级P p对称性，发现包含C-H ... F相互作用。

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