International Journal of Inorganic Chemistry

Research Article

Syntheses and Crystal Structures of Two Transition Metal Complexes (M = Mn and Co) Containing Malonate and Reduced Imino Nitroxide Radicals

Table 1

Summary of the crystallographic data and collections for two complexes.
Complex 1Complex 2
Empirical formulaC27H34ClCoN6O10C27H36MnN6O7
Formula weight696.98611.56
Crystal system, space groupMonoclinic, C2 Monoclinic, C2
Unit cell dimensions 𝑎 = 1 7 . 0 0 4 ( 9 )  Å 𝑏 = 1 0 . 7 5 3 ( 5 )  Å 𝑐 = 9 . 2 0 7 ( 5 )  Å 𝛽 = 1 3 . 8 5 6 ( 8 ) ∘ 𝑎 = 1 6 . 7 2 1 ( 5 )  Å 𝑏 = 1 0 . 8 9 7 ( 5 )  Å 𝑐 = 9 . 2 5 3 ( 3 )  Åβ = 120.807(6)°
Volume1539.6(14)  Å31448.1(9) Å3
𝑍 , Calculated density2, 1.504 Mg/m32, 1.403 Mg/m3
Absorption coefficient0.710 mm-10.511 mm-1
F(000)724642
Crystal size0.18 × 0.16 × 0.14 mm30.24 × 0.22 × 0.18 mm3
𝜃 range for data collection2.30 to 25.10˚2.35 to 25.01˚
Limiting indices − 2 0 ≤ ℎ ≤ 2 0 , − 1 2 ≤ 𝑘 ≤ 1 1 , − 9 ≤ 𝑙 ≤ 1 0 − 1 9 ≤ ℎ ≤ 1 4 , − 1 2 ≤ 𝑘 ≤ 1 2 , − 1 1 ≤ 𝑙 ≤ 1 1
Reflections collected/unique3755/2253 ( 𝑅 (int) = 0 . 0 3 1 8 )3730/2519 ( 𝑅 ( i n t ) = 0 . 0 1 5 4 )
Completeness to 𝜃 = 2 5 . 1 0 95.4%100.0%
Absorption correctionSemi-empirical from equivalentsSemi-empirical from equivalents
Max. and min. transmission1.000000 and 0.7116021.000000 and 0.754606
Refinement methodFull-matrix least-squares on 𝐹 2 Full-matrix least-squares on 𝐹 2
Data/restraints/parameters2253/47/2282519/2/190
Goodness-of-fit on F 21.0371.107
Final 𝑅 indices ( 𝐼 > 2 𝜎 ( 𝐼 )) 𝑅 1 = 0 . 0 5 0 2 , 𝑤 𝑅 2 = 0 . 1 2 5 7 𝑅 1 = 0 . 0 4 0 1 , 𝑤 𝑅 2 = 0 . 1 0 6 9
𝑅 indices (all data) 𝑅 1 = 0 . 0 5 8 3 , 𝑤 𝑅 2 = 0 . 1 3 1 1 𝑅 1 = 0 . 0 4 1 8 , 𝑤 𝑅 2 = 0 . 1 0 9 1
Absolute structure parameter0.00(3)0.0(2)
Largest diff. peak and hole1.136 and −0.285 e.A-30.745 and −0.294 e.A-3