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Organometallics

Volumn 26, Issue 1, 2007, Pages 26-29

New structural forms of organostannoxane macrocycle networks

(3) Chandrasekhar, Vadapalli a Thirumoorthi, Ramalingam a Azhakar, Ramachandran a

a INDIAN INSTITUTE OF TECHNOLOGY KANPUR (India)

Author keywords

[No Author keywords available]

Indexed keywords

CARBOXYLIC ACIDS; COMPLEXATION; ORGANOMETALLICS; POTASSIUM COMPOUNDS;

DIBENZYLTIN DICHLORIDE; ORGANOSTANNOXANE MACROCYCLE NETWORKS; POTASSIUM HYDROXIDE; PYRAZOLE-3,5-DICARBOXYLIC ACID;

TIN COMPOUNDS;

EID: 33846254123 PISSN: 02767333 EISSN: None Source Type: Journal
DOI: 10.1021/om061010x Document Type: Article

Times cited : (36)

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28
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- Synthesis of 1: pyrazole-3,5-dicarboxylic acid (0.039 g, 0.22 mmol) was added to a solution of KOH (0.037 g, 0.67 mmol) in a 30 mL mixture of ethanol and water (2:1, and this mixture was stirred for 5 min to obtain a clear solution. At this stage (Bz)2SnCl2 (0.33 g, 0.89 mmol) was added. The reaction mixture was stirred for a further 3 h at room temperature and then heated to reflux for 3 h. It was cooled and filtered. The solid precipitate that was obtained was washed with water (3 ×10 mL, This was sparingly soluble in organic solvents and could be recrystallized from a mixture of tetrahydrofuran, ethanol, and methanol (4:2:1) to afford colorless crystals of 1 (0.18 g, 92% yield, Mp: >250 °C dec. Anal. Calcd for C 132H126-Sn8O22Cl2N 8 1, C, 49.59; H, 3.97; N, 3.50. Found: C, 49.52; H, 3.86; N, 2.98
- 8 (1): C, 49.59; H, 3.97; N, 3.50. Found: C, 49.52; H, 3.86; N, 2.98.

29
- 33846232805
- Crystal data for 1: monoclinic; P2l/c; a, 23.398(5) Å, b, 17.539-(5) Å, c, 32.266(5) A; β= 107.938(5)°; V, 12598(5) Å3; T, 100(2) K; Z, 4; DCalcd, 0.422 mg m -3; crystal dimensions 0.2 × 0.3 × 0.2 mm; 2θmax, 25.03°; 65 147 reflections measured; 22 138 unique reflections (I > 2σ(I, 1472 parameters; R1, 0.0696; wR2, 0.1512. Crystal data for 2: triclinic; P1; a, 13.717(2) Å, b, 17.571(3) Å c, 19.095(3) Å; α, 96.546(4, β, 93.933(4, y, 93.317(4, γ V, 4551.7(13) Å3; T= 100(2) K; Z, 1, Dcalcd, 0.792 mg m-3; crystal dimensions 0.2 × 0.3 × 0.2 mm; 2θmax, 25.03°; 23 865 reflections measured; 15 769 unique reflections (I > 2σI, 1028 parameters; R1, 0.0793; wR2, 0.1680
- max = 25.03°; 23 865 reflections measured; 15 769 unique reflections (I > 2σ(I)); 1028 parameters; R1 = 0.0793; wR2 = 0.1680.

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32
- 33846238237
- 5, 20 °C): δ-302.40, -313.88. -422.83 ppm.
- 5, 20 °C): δ-302.40, -313.88. -422.83 ppm.

* 이 정보는 Elsevier사의 SCOPUS DB에서 KISTI가 분석하여 추출한 것입니다.