Structural aspect of the reaction of copper(I) chloride with 1-cyanobuta-1,3-diene

Mys’kiv, М. G.; Oliinik, Volodymyr; Zavalii, P. Yu.

doi:10.1007/bf00748832

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“…3). On the contrary, in the molecular π-complex [CuCl(HOCH 2 C≡CCH 2 OH)] [1], the ≡ëëç 2 é-ç···é(ç)ëç 2 ë≡ hydrogen bonds are formed between the neighboring molecules of 2-butyne-1,4-diol, although the conformation parameter of two halves (H-O-Cç 2 -C≡) of the ligand molecule are also different.…”

Section: Resultsmentioning

confidence: 90%

“…The bond angles C(1)-C(2)≡C(3) and C(2)≡C(3)-C(4) in (I) are 166.2(8)° and 163.7(9)°, respectively, while the C(2)≡C(3) bond, which is π-coordinated on a metal center, is elongated to 1.223(11) Å (Table 3) (in ä[CuBr 2 (HOCH 2 C≡CCH 2 OH)] [1], the length of this bond is 1.24(1) Å).…”

Section: Resultsmentioning

confidence: 98%

“…By replacing KBr by NH 4 Cl and then by RbCl in the above system, we obtained crystals of π -complex NH 4 [ CuCl 2 ( HOCH 2 C ≡ CCH 2 OH )] [2] and of two dimorphic complexes Rb [ CuCl 2 ( HOCH 2 C ≡ CCH 2 OH )] [3]. One dimorphic complex is also isostructural to the potassium [1] and ammonium [2] analogs.…”

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confidence: 99%

“…The crystals of molecular [CuCl ( HOCH 2 C ≡ CCH 2 OH ) and anionic ä[ CuBr 2 ( HOCH 2 C ≡ CCH 2 OH )] π -complexes were synthesized while studying the system ä Br -CuCl -H 2 O -HOCH 2 C ≡ CCH 2 OH [1] and were investigated by X-ray diffraction analysis. By replacing KBr by NH 4 Cl and then by RbCl in the above system, we obtained crystals of π -complex NH 4 [ CuCl 2 ( HOCH 2 C ≡ CCH 2 OH )] [2] and of two dimorphic complexes Rb [ CuCl 2 ( HOCH 2 C ≡ CCH 2 OH )] [3].…”

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π-Complexes of Cu(I) with Alkynes. Synthesis and Crystal Structure of Cs[CuCl2(HOCH2C≡CCH2OH)] ⋅ H2O

2005

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This work continues systematic studies of the structure of π -complexes of Cu(I) halides with 2-butyne-1,4-diol formed in concentrated aqueous solutions of CuCl and MCl (where M are cations of the alkali metals, ammonium, and of organic amines).The crystals of molecular [CuCl ( HOCH 2 C ≡ CCH 2 OH ) and anionic ä[ CuBr 2 ( HOCH 2 C ≡ CCH 2 OH )] π -complexes were synthesized while studying the system ä Br -CuCl -H 2 O -HOCH 2 C ≡ CCH 2 OH [1] and were investigated by X-ray diffraction analysis. By replacing KBr by NH 4 Cl and then by RbCl in the above system, we obtained crystals of π -complex NH 4 [ CuCl 2 ( HOCH 2 C ≡ CCH 2 OH )] [2] and of two dimorphic complexes Rb [ CuCl 2 ( HOCH 2 C ≡ CCH 2 OH )] [3]. One dimorphic complex is also isostructural to the potassium [1] and ammonium [2] analogs.In order to establish the effect of an outer-sphere å + cation on the structure of anionic π -complexes of Cu(I) with 2-butyne-1,4-diol, we determined the structure of the crystals Cs [ CuCl 2 (EXPERIMENTAL Synthesis. Crystals I were synthesized by the direct reaction of Cu(I) chloride with 2-butyne-1,4-diol in a saturated aqueous solution of CsCl. A saturated aqueous solution of CsCl (0.01 mol, 1.7 g) was prepared at ~90° C and CuCl (0.01 mol, 1.0 g) was dissolved in it. Then, HOCH 2 C ≡ CCH 2 OH (0.01 mol, 0.9 g) was added and the solution was cooled to room temperature. The crystals of complex I formed as almost colorless triclinic prisms. The crystal density was measured by flotation method in a chloroform-bromoform mixture.X-ray diffraction analysis of single crystals I , which were preliminarily studied by photomethod, was performed on a single-crystal DARCh automated diffractometer ( åÓ K α radiation, θ /2 θ -scan mode). The crystallographic parameters and details of the data collection for complex I are given in Table 1.The structure was solved by the direct methods with CSD program package [4]. All non-hydrogen atoms were localized and refined by the least-squares method in isotropic approximation; the absorption correction was applied with DIFABS program. The hydrogen atoms were located geometrically. The final structure refinement was performed for non-hydrogen atoms in anisotropic (for the H atoms, in isotropic) approximation.The coordinates of atoms and their thermal parameters are listed in Table 2. RESULTS AND DISCUSSIONThe structure of complex I is shown in Fig. 1. Like the previously studied anionic π -complexes M [ CuCl 2 ( HOCH 2 C ≡ CCH 2 OH )] (M = , K + [2], Rb + [3]) and ä[ CuBr 2 ( HOCH 2 C ≡ CCH 2 OH )] [1], compound I consists of individual complex anions [ CuCl 2 ( HOCH 2 C ≡ CCH 2 OH )] -(Fig. 2) and hydrated Cs NH 4 + Abstract -Crystals of anionic π -complex Cs [ CuCl 2 ( HOCH 2 C≡CCH 2 OH)] · H 2 O were synthesized by reaction of 2-butyne-1,4-diol with CuCl in a saturated aqueous solution of CsCl at 90°C and studied by X-ray diffraction analysis. The crystals are triclinic (space group ; a = 10.155(4) Å, b = 7.828(4) Å, c = 7.115(3) Å, α = 102.62(4)°, β = 100.77(3)°, γ = 106.71(4)°, V = 509(1...

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Section: Resultsmentioning

confidence: 90%

Section: Resultsmentioning

confidence: 98%

mentioning

confidence: 99%

mentioning

confidence: 99%

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