Dimeric complexes containing the [Fe2S2]2+ cores coordinated by non-sulfur terminal ligands. Synthesis, structural characterization, and spectroscopic properties of [Et4N]2[Fe2S2(o,o′-C 12H8O2)2], [Et4N] ...

A. Salifoglou, A. Simopoulos, A. Kostikas, R. W. Dunham, Mercouri G Kanatzidis, D. Coucouvanis

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Abstract

Full title: Dimeric complexes containing the [Fe2S2]2+ cores coordinated by non-sulfur terminal ligands. Synthesis, structural characterization, and spectroscopic properties of [Et4N]2[Fe2S2(o,o′-C 12H8O2)2], [Et4N]2[Fe2S2(C4H 4N)4], and [Et4N]2[Fe2S2(O-o-C 6H4CH(n-C4H9)NHC6H 4-o-S)2] and the Structure of [Ph4P]2[Fe2S2(OC6H 4-p-CH3)4]. The synthesis and spectroscopic characterization of the [Fe2S2L4]2- clusters (L2 = o,o′-C12H8O22-, -O-o-C6H4CH(n-Bu)NHC6H 4-o-S-; L = -OC6H4-p-CH3, C4H4N-) are reported. The crystal and molecular structures of (Et4N)2[Fe2S2(o,o′-C 12H8O2)2] (I), (Et4N)2[Fe2S2(C4H 4N)4] (II), (Et4N)2[Fe2S2(O-o-C 6H4CH(n-Bu)NHC6H4-o-S)2] (III), and (Ph4P)2[Fe2S2(OC6H 4-p-CH3)4] (IV) are described in detail. I crystallizes in the monoclinic space group C2/c, with cell dimensions a = 11.500 (2) Å, b = 13.541 (3) Å, c = 26.612 (5) Å, β = 92.25 (1)°, and Z = 4. II crystallizes in monoclinic space group P21/n, with cell dimensions a = 9.689 (3) Å, b = 16.362 (2) Å, c = 11.910 (5) Å, β = 97.74 (3)°, and Z = 2. III crystallizes in the monoclinic space group P21/c, with cell dimensions a = 14.878 (4) Å, b = 9.585 (3) Å, c = 18.950 (6) Å, β = 95.59 (2)°, and Z = 2, and IV crystallizes in the monoclinic space group P21/a, with cell dimensions a = 16.308 (5) Å, b = 16.674 (6) Å, c = 24.456 (9) Å, β = 91.13 (3)°, and Z = 4. Intensity data for I-IV were collected on a four-circle computer-controlled diffractometer with use of the θ-2θ scan technique. All four structures were solved by conventional methods from 2739, 1736, 2086 and 3632 reflections for I-IV, respectively. The structures were refined by full-matrix least-squares techniques (310 parameters for I, 173 parameters for II, 280 parameters for III, and 385 parameters for IV) to final R values of 0.033 (I), 0.069 (II), 0.065 (III), and 0.074 (IV). Complexes I-IV contain the planar [Fe2S2]2+ cores coordinated fully or partially by non-sulfur terminal ligands. The Fe⋯Fe distance in the centrosymmetric dianions ranges from 2.677 (3) Å in II to 2.749 (24) Å in IV. The Fe-O distances are 1.894 (2) (I), 1.921 (11) (III), and 1.870 (12) Å (IV), and the Fe-N distance in II is 1.97 (5) Å. Structural comparisons with the already reported thiolate dimers [Fe2S2L4]2- (L = -SAr; L2 = S2-o-xyl2-) are reported. The electronic, Mössbauer, cyclic voltammetric, and proton magnetic resonance properties of the new dimers are discussed in detail. A comparison of these properties with the available data on the Rieske [Fe2S2] centers is presented and certain conclusions are drawn concerning future design of synthetic analogues.

Original languageEnglish
Pages (from-to)3394-3406
Number of pages13
JournalInorganic Chemistry
Volume27
Issue number19
Publication statusPublished - 1988

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Dimeric complexes containing the [Fe2S2]2+ cores coordinated by non-sulfur terminal ligands. Synthesis, structural characterization, and spectroscopic properties of [Et4N]2[Fe2S2(o,o′-C 12H8O2)2], [Et4N] ... / Salifoglou, A.; Simopoulos, A.; Kostikas, A.; Dunham, R. W.; Kanatzidis, Mercouri G; Coucouvanis, D.

In: Inorganic Chemistry, Vol. 27, No. 19, 1988, p. 3394-3406.

Research output: Contribution to journalArticle

@article{2bf789885e4c4a4ebeb927c44a635434,
title = "Dimeric complexes containing the [Fe2S2]2+ cores coordinated by non-sulfur terminal ligands. Synthesis, structural characterization, and spectroscopic properties of [Et4N]2[Fe2S2(o,o′-C 12H8O2)2], [Et4N] ...",
abstract = "Full title: Dimeric complexes containing the [Fe2S2]2+ cores coordinated by non-sulfur terminal ligands. Synthesis, structural characterization, and spectroscopic properties of [Et4N]2[Fe2S2(o,o′-C 12H8O2)2], [Et4N]2[Fe2S2(C4H 4N)4], and [Et4N]2[Fe2S2(O-o-C 6H4CH(n-C4H9)NHC6H 4-o-S)2] and the Structure of [Ph4P]2[Fe2S2(OC6H 4-p-CH3)4]. The synthesis and spectroscopic characterization of the [Fe2S2L4]2- clusters (L2 = o,o′-C12H8O22-, -O-o-C6H4CH(n-Bu)NHC6H 4-o-S-; L = -OC6H4-p-CH3, C4H4N-) are reported. The crystal and molecular structures of (Et4N)2[Fe2S2(o,o′-C 12H8O2)2] (I), (Et4N)2[Fe2S2(C4H 4N)4] (II), (Et4N)2[Fe2S2(O-o-C 6H4CH(n-Bu)NHC6H4-o-S)2] (III), and (Ph4P)2[Fe2S2(OC6H 4-p-CH3)4] (IV) are described in detail. I crystallizes in the monoclinic space group C2/c, with cell dimensions a = 11.500 (2) {\AA}, b = 13.541 (3) {\AA}, c = 26.612 (5) {\AA}, β = 92.25 (1)°, and Z = 4. II crystallizes in monoclinic space group P21/n, with cell dimensions a = 9.689 (3) {\AA}, b = 16.362 (2) {\AA}, c = 11.910 (5) {\AA}, β = 97.74 (3)°, and Z = 2. III crystallizes in the monoclinic space group P21/c, with cell dimensions a = 14.878 (4) {\AA}, b = 9.585 (3) {\AA}, c = 18.950 (6) {\AA}, β = 95.59 (2)°, and Z = 2, and IV crystallizes in the monoclinic space group P21/a, with cell dimensions a = 16.308 (5) {\AA}, b = 16.674 (6) {\AA}, c = 24.456 (9) {\AA}, β = 91.13 (3)°, and Z = 4. Intensity data for I-IV were collected on a four-circle computer-controlled diffractometer with use of the θ-2θ scan technique. All four structures were solved by conventional methods from 2739, 1736, 2086 and 3632 reflections for I-IV, respectively. The structures were refined by full-matrix least-squares techniques (310 parameters for I, 173 parameters for II, 280 parameters for III, and 385 parameters for IV) to final R values of 0.033 (I), 0.069 (II), 0.065 (III), and 0.074 (IV). Complexes I-IV contain the planar [Fe2S2]2+ cores coordinated fully or partially by non-sulfur terminal ligands. The Fe⋯Fe distance in the centrosymmetric dianions ranges from 2.677 (3) {\AA} in II to 2.749 (24) {\AA} in IV. The Fe-O distances are 1.894 (2) (I), 1.921 (11) (III), and 1.870 (12) {\AA} (IV), and the Fe-N distance in II is 1.97 (5) {\AA}. Structural comparisons with the already reported thiolate dimers [Fe2S2L4]2- (L = -SAr; L2 = S2-o-xyl2-) are reported. The electronic, M{\"o}ssbauer, cyclic voltammetric, and proton magnetic resonance properties of the new dimers are discussed in detail. A comparison of these properties with the available data on the Rieske [Fe2S2] centers is presented and certain conclusions are drawn concerning future design of synthetic analogues.",
author = "A. Salifoglou and A. Simopoulos and A. Kostikas and Dunham, {R. W.} and Kanatzidis, {Mercouri G} and D. Coucouvanis",
year = "1988",
language = "English",
volume = "27",
pages = "3394--3406",
journal = "Inorganic Chemistry",
issn = "0020-1669",
publisher = "American Chemical Society",
number = "19",

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TY - JOUR

T1 - Dimeric complexes containing the [Fe2S2]2+ cores coordinated by non-sulfur terminal ligands. Synthesis, structural characterization, and spectroscopic properties of [Et4N]2[Fe2S2(o,o′-C 12H8O2)2], [Et4N] ...

AU - Salifoglou, A.

AU - Simopoulos, A.

AU - Kostikas, A.

AU - Dunham, R. W.

AU - Kanatzidis, Mercouri G

AU - Coucouvanis, D.

PY - 1988

Y1 - 1988

N2 - Full title: Dimeric complexes containing the [Fe2S2]2+ cores coordinated by non-sulfur terminal ligands. Synthesis, structural characterization, and spectroscopic properties of [Et4N]2[Fe2S2(o,o′-C 12H8O2)2], [Et4N]2[Fe2S2(C4H 4N)4], and [Et4N]2[Fe2S2(O-o-C 6H4CH(n-C4H9)NHC6H 4-o-S)2] and the Structure of [Ph4P]2[Fe2S2(OC6H 4-p-CH3)4]. The synthesis and spectroscopic characterization of the [Fe2S2L4]2- clusters (L2 = o,o′-C12H8O22-, -O-o-C6H4CH(n-Bu)NHC6H 4-o-S-; L = -OC6H4-p-CH3, C4H4N-) are reported. The crystal and molecular structures of (Et4N)2[Fe2S2(o,o′-C 12H8O2)2] (I), (Et4N)2[Fe2S2(C4H 4N)4] (II), (Et4N)2[Fe2S2(O-o-C 6H4CH(n-Bu)NHC6H4-o-S)2] (III), and (Ph4P)2[Fe2S2(OC6H 4-p-CH3)4] (IV) are described in detail. I crystallizes in the monoclinic space group C2/c, with cell dimensions a = 11.500 (2) Å, b = 13.541 (3) Å, c = 26.612 (5) Å, β = 92.25 (1)°, and Z = 4. II crystallizes in monoclinic space group P21/n, with cell dimensions a = 9.689 (3) Å, b = 16.362 (2) Å, c = 11.910 (5) Å, β = 97.74 (3)°, and Z = 2. III crystallizes in the monoclinic space group P21/c, with cell dimensions a = 14.878 (4) Å, b = 9.585 (3) Å, c = 18.950 (6) Å, β = 95.59 (2)°, and Z = 2, and IV crystallizes in the monoclinic space group P21/a, with cell dimensions a = 16.308 (5) Å, b = 16.674 (6) Å, c = 24.456 (9) Å, β = 91.13 (3)°, and Z = 4. Intensity data for I-IV were collected on a four-circle computer-controlled diffractometer with use of the θ-2θ scan technique. All four structures were solved by conventional methods from 2739, 1736, 2086 and 3632 reflections for I-IV, respectively. The structures were refined by full-matrix least-squares techniques (310 parameters for I, 173 parameters for II, 280 parameters for III, and 385 parameters for IV) to final R values of 0.033 (I), 0.069 (II), 0.065 (III), and 0.074 (IV). Complexes I-IV contain the planar [Fe2S2]2+ cores coordinated fully or partially by non-sulfur terminal ligands. The Fe⋯Fe distance in the centrosymmetric dianions ranges from 2.677 (3) Å in II to 2.749 (24) Å in IV. The Fe-O distances are 1.894 (2) (I), 1.921 (11) (III), and 1.870 (12) Å (IV), and the Fe-N distance in II is 1.97 (5) Å. Structural comparisons with the already reported thiolate dimers [Fe2S2L4]2- (L = -SAr; L2 = S2-o-xyl2-) are reported. The electronic, Mössbauer, cyclic voltammetric, and proton magnetic resonance properties of the new dimers are discussed in detail. A comparison of these properties with the available data on the Rieske [Fe2S2] centers is presented and certain conclusions are drawn concerning future design of synthetic analogues.

AB - Full title: Dimeric complexes containing the [Fe2S2]2+ cores coordinated by non-sulfur terminal ligands. Synthesis, structural characterization, and spectroscopic properties of [Et4N]2[Fe2S2(o,o′-C 12H8O2)2], [Et4N]2[Fe2S2(C4H 4N)4], and [Et4N]2[Fe2S2(O-o-C 6H4CH(n-C4H9)NHC6H 4-o-S)2] and the Structure of [Ph4P]2[Fe2S2(OC6H 4-p-CH3)4]. The synthesis and spectroscopic characterization of the [Fe2S2L4]2- clusters (L2 = o,o′-C12H8O22-, -O-o-C6H4CH(n-Bu)NHC6H 4-o-S-; L = -OC6H4-p-CH3, C4H4N-) are reported. The crystal and molecular structures of (Et4N)2[Fe2S2(o,o′-C 12H8O2)2] (I), (Et4N)2[Fe2S2(C4H 4N)4] (II), (Et4N)2[Fe2S2(O-o-C 6H4CH(n-Bu)NHC6H4-o-S)2] (III), and (Ph4P)2[Fe2S2(OC6H 4-p-CH3)4] (IV) are described in detail. I crystallizes in the monoclinic space group C2/c, with cell dimensions a = 11.500 (2) Å, b = 13.541 (3) Å, c = 26.612 (5) Å, β = 92.25 (1)°, and Z = 4. II crystallizes in monoclinic space group P21/n, with cell dimensions a = 9.689 (3) Å, b = 16.362 (2) Å, c = 11.910 (5) Å, β = 97.74 (3)°, and Z = 2. III crystallizes in the monoclinic space group P21/c, with cell dimensions a = 14.878 (4) Å, b = 9.585 (3) Å, c = 18.950 (6) Å, β = 95.59 (2)°, and Z = 2, and IV crystallizes in the monoclinic space group P21/a, with cell dimensions a = 16.308 (5) Å, b = 16.674 (6) Å, c = 24.456 (9) Å, β = 91.13 (3)°, and Z = 4. Intensity data for I-IV were collected on a four-circle computer-controlled diffractometer with use of the θ-2θ scan technique. All four structures were solved by conventional methods from 2739, 1736, 2086 and 3632 reflections for I-IV, respectively. The structures were refined by full-matrix least-squares techniques (310 parameters for I, 173 parameters for II, 280 parameters for III, and 385 parameters for IV) to final R values of 0.033 (I), 0.069 (II), 0.065 (III), and 0.074 (IV). Complexes I-IV contain the planar [Fe2S2]2+ cores coordinated fully or partially by non-sulfur terminal ligands. The Fe⋯Fe distance in the centrosymmetric dianions ranges from 2.677 (3) Å in II to 2.749 (24) Å in IV. The Fe-O distances are 1.894 (2) (I), 1.921 (11) (III), and 1.870 (12) Å (IV), and the Fe-N distance in II is 1.97 (5) Å. Structural comparisons with the already reported thiolate dimers [Fe2S2L4]2- (L = -SAr; L2 = S2-o-xyl2-) are reported. The electronic, Mössbauer, cyclic voltammetric, and proton magnetic resonance properties of the new dimers are discussed in detail. A comparison of these properties with the available data on the Rieske [Fe2S2] centers is presented and certain conclusions are drawn concerning future design of synthetic analogues.

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M3 - Article

VL - 27

SP - 3394

EP - 3406

JO - Inorganic Chemistry

JF - Inorganic Chemistry

SN - 0020-1669

IS - 19

ER -