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Original Articles

THE PHENOMENON OF CONGLOMERATE CRYSTALLIZATION. PART 43. THE CRYSTALLIZATION BEHAVIOR OF K[cis-α-Co(N-N′-Et2-Edda)(NO2)2] · 2H2O (I), {CS[cis-α-Co(Edda)(NO2)2]}2 · 3H2O (II), Rb[cis-α-Co(Edda)(NO2)2 · H2O (III) and NH4[cis-α-Co(Edda)(NO2)2] · 2H2O (IV)

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Pages 1-26 | Received 24 Oct 1995, Published online: 22 Sep 2006
 

Abstract

K[cis-α-Co(Et2-edda)(NO2)2] · 2H2O (I), CoKO10N4C10H22, crystallizes in the space group P21/n(No. 14), with lattice constants: a = 7.339(2), b = 15.750(3), c = 15.492(4) Å and β 101.65(2)°; V = 1753.86Å3 and d(calc; MW = 456.34, Z = 4) = 1.728 g-cm−3. A total of 3335 data were collected over the range of 4° ≤ 2θ ≤ 50°; of these, 2553 (independent and with I > 3σ(I)) were used in the structural analysis. Data were corrected for absorption (μ = 12.688 cm−1) and the transmission coefficients ranged from 0.8860 to 0.9997. Final values of the residuals were R(F) = 0.0275 and Rw (F) = 0.0301. The anions of the racemic pairs in the unit cell have the chiroptical symbols A(δΛδ) and Δ(ΛδΛ).

{Cs[cis-α-Co(edda)(NO2)2]}2 · 3H2O (II), Cs2Co2O19N8C8H18, crystallizes in the space group C2/c(No. 15), with lattice constants: a = 19.304(6), b = 10.992(4), c = 13.809 (5) Å and β = 106.42(3)°; V = 2827.11 Å3 and d(calc; MW = 913.95 Z = 4) = 2.147 g-cm−1. A total of 4192 data were collected over the range of 4° ≤ 2θ ≤ 60°; of these, 2837 (independent and with I > 2.5σ(I)) were used in the structural analysis. Data were corrected for absorption (μ = 37.70 cm−1) and the transmission coefficients ranged from 0.2362 to 0.4458. Final values of the residuals were R(F) = 0.034 and Rw (F) = 0.035. The anions of the racemic pairs in the unit cell have the chiroptical symbols Δ(ΛδΛ) and Λ(δΛδ).

Rb[cis-α-Co(edda)(NO2)2] · H2O (III), RbCoO9N4C6H12, crystallizes in the space group P 1 (No. 2), with lattice constants: a = 7.348 (1), b = 9.986(2), c = 11.102 (3) Å, α = 63.36(2)°, β = 66.23(2)° and γ = 75.79(2)°; V = 664.27 Å3 and d(calc; MW = 428.58, Z = 2) = 2.143 g-cm−3. A total of 2496 reflections were collected over the range of 4° ≤ 2θ ≤ 60°; of these, 1764 (independent and with I > 2.5σ(I)) were used in the structural analysis. Data were corrected for absorption (μ = 48.80 cm−1) and the transmission coefficients ranged from 0.1891 to 0.3565. Final values of the residuals were R(F) = 0.045 and R(F) = 0.052. The anions of the racemic pairs in the unit cell have the chiroptical symbols Δ(ΛδΛ) and Λ(δΛδ).

NH4[cis-α-Co(edda)(NO2)2] · 2H2O (IV), CoO10N5C6H18, crystallizes in the space group C2/c(No. 15), with lattice constants: a = 23.240 (14), b = 7.101 (9), c = 20.948 (17) Å and β = 122.11(7)°; V = 2928.18 Å3 and d(calc; MW = 379.17, Z = 8) = 1.720 g-cm−3. A total of 3474 data were collected over the range of 4° < 2θ ≤ 55° of these, 1639 (independent and with I ≥ 2.5σ(I)) were used in the structural analysis. Data were corrected for absorption (μ = 12.30 cm−1) and the transmission coefficients ranged from 0.6733 to 0.7570. Final values of the residuals were R(F) = 0.045 and Rw (F) = 0.049. The anions of the racemic pairs in the unit cell have the chiroptical symbols Λ(δΛδ) and Δ(ΛδΛ).

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