Synthesis and crystal structure of [Zn₆Br₄(C₉H₁₈NO)₄(OH)₄]·2C₃H₆O₂

Abstract

<jats:p>The complete molecule of the hexametallic title complex, namely, tetrabromidotetra-μ-hydroxido-hexakis[μ-2-methyl-3-(pyrrolidin-1-yl)propan-2-olato]hexazinc(II) acetone disolvate, [Zn<jats:sub>6</jats:sub>Br<jats:sub>4</jats:sub>(C<jats:sub>9</jats:sub>H<jats:sub>18</jats:sub>NO)<jats:sub>4</jats:sub>(OH)<jats:sub>4</jats:sub>]·2C<jats:sub>3</jats:sub>H<jats:sub>6</jats:sub>O<jats:sub>2</jats:sub>, is generated by a crystallographic centre of symmetry. Two of the unique zinc atoms adopt distorted ZnO<jats:sub>2</jats:sub>NBr tetrahedral coordination geometries and the other adopts a ZnO<jats:sub>3</jats:sub>N tetrahedral arrangement. Both unique alkoxide ligands are <jats:italic>N</jats:italic>,<jats:italic>O</jats:italic>-chelating and both hydroxide ions are μ<jats:sup>2</jats:sup> bridging. The crystal structure displays an O—H...O hydrogen bond between a μ<jats:sup>2</jats:sup>-OH group and an acetone solvent molecule. The Hirshfeld surface has been calculated and is described.</jats:p>

Synthesis of Heteroleptic Zinc Complexes Containing Aminoalkoxide and β‐Diketonate Ligands

“…The bite angles of O−Zn‐N in aminoalkoxide were 81.86(6)° ( 1 ), 81.81(6)° ( 2 ), 84.11(5)° ( 3 ), 81.52(6)° ( 4 ), and 84.22(11)° ( 6 ); these were almost similar to that previously reported zinc complexes (86.91‐88.54°) [22] . The bite angles of O−Zn‐O in β ‐diketonate were 87.91(5)° (1), 88.77(6)° (2), 85.58(5)° (3), 88.38(6)° (4), and 85.54(10)° (6), which were in the range of known β ‐diketonate Zn complexes (89.42°) [23] .…”

“…The Zn−O bond lengths with the aminoalkoxide ligands were determined to be 2.0689(13) Å ( 1 ), 2.0711(13) Å ( 2 ), 2.0523(12) Å ( 3 ), 2.0632(14) Å ( 4 ), and 2.051(3) Å ( 6 ). These were slightly longer than that in previously reported zinc complexes (1.9401‐1.9593 Å) [22] . The coordinated Zn−N bond distances with the aminoalkoxide ligands were 2.1808(17) Å ( 1 ), 2.1659(17) Å ( 2 ), 2.1097(16) Å ( 3 ), 2.1887(18) Å ( 4 ), and 2.114(3) Å ( 6 ); these Zn←N bond lengths were similar to that previously reported zinc complexes (2.1058–2.1358 Å) [22] …”

“…The bite angles of OÀ Zn-N in aminoalkoxide were 81.86(6)°( 1), 81.81(6)°(2), 84.11(5)°(3), 81.52(6)°(4), and 84.22(11)°(6); these were almost similar to that previously reported zinc complexes (86.91-88.54°). [22] The bite angles of OÀ Zn-O in βdiketonate were 87.91(5)°(1), 88.77(6)°(2), 85.58(5)°(3), 88.38(6)°(4), and 85.54(10)°(6), which were in the range of known β-diketonate Zn complexes (89.42°). [23] The oxygen atoms of the β-diketonate ligands (O1 or O2) and aminoalkoxide ligands (O3) were situated in the axial positions with bond angles of 166.29(6)°(1), 164.94(6)°(2), 169.50(5)°(3), 165.10( 7)°(4), and 167.52(10)°(6).…”

“…These were slightly longer than that in previously reported zinc complexes (1.9401-1.9593 Å). [22] The coordinated ZnÀ N bond Scheme 1. Synthesis of complexes 1-6.…”

“…N bond lengths were similar to that previously reported zinc complexes (2.1058-2.1358 Å). [22] The ZnÀ O bond lengths between the central zinc ion and oxygen atom of β-diketonate ligands were 2.0192(13) Å (1), 2.0395( 14) Å (2), 2.0784(13) Å (3), 2.0245(15) Å (4), and 2.079(2) Å (6), which were in the range of known β-diketonate zinc complexes (2.022-2.096 Å). [23] The Zn⋅⋅⋅Zn distances were 2.9531(5) Å (1), 2.9752(5) Å (2), 2.9425(4) Å (3), 2.9603(4) Å (4), and 2.9225(8) Å (6).…”