Synthesis, Crystal Structure and Magnetic Properties of Tetranuclear MnⅡ2MnⅢ2 Complexes Based on 2-(Hydroxymethyl)-N-methylimidazole†

doi:10.7503/cjcu20130671

Abstract

Abstract:

Three new 2-(hydroxymethyl)-N-methylimidazole-bridged tetranuclear Mn^Ⅱ₂Mn^Ⅲ₂ complexes [Mn₄(hmmi)₆(DMF)₂(N₃)₂](ClO₄)₂(1), [Mn₄(hmmi)₆(H₂O)₂(N₃)₂](ClO₄)₂(2) and [Mn₄(hmmi)₆Cl₄]·6CH₃CN(3·6CH₃CN)[Hhmmi=2-(hydroxymethyl)-N-methylimidazole] were synthesized, and their crystal structures and magnetic properties were studied. In the mixed-valent [Mn₄]²⁺ cores for complexes 1—3, Mn^Ⅱ are located at the sides, and Mn^Ⅲ in the middle. Best fit to the experimental data for complexes 1—3 suggests the presence of ferromagnetic coupling for Mn^Ⅲ-Mn^Ⅲ, while weak ferromagnetic or antiferromagnetic coupling for Mn^Ⅲ-Mn^Ⅱ or intermolecular interaction.

Key words: 2-(Hydroxymethyl)-N-methylimidazole, Manganese, Tetranuclear complex, Magnetism, Mixed-valent

CLC Number:

O614

TrendMD:

SHI Wenbo, KOU Huizhong. Synthesis, Crystal Structure and Magnetic Properties of Tetranuclear Mn^Ⅱ₂Mn^Ⅲ₂ Complexes Based on 2-(Hydroxymethyl)-N-methylimidazole^†[J]. Chem. J. Chinese Universities, 2014, 35(1): 12.

Figures/Tables 12

Table 1 Crystallographic data for complexes 1—3

Compound	1	2	3·6CH₃CN
Empirical formula	C₃₆H₅₆ $N 2 0$ O₁₆Cl₂Mn₄	C₃₀ $H 4 6$ N₁₈O₁₆Cl₂Mn₄	$C 4 2$ H₆₀N₁₈O₆Cl₄Mn₄
Formula weight	1315.67	1205.51	1274.64
Crystal system	Monoclinic	Monoclinic	Triclinic
Space group	C2/c	P2₁/c	P-1
a/nm	2.8773(4)	1.2276(2)	1.0440(3)
b/nm	1.8427(2)	1.0738(2)	1.1281(4)
c/nm	1.0991(2)	1.8502(2)	1.3646(3)
α/(°)	90	90	80.57(1)
β/(°)	109.77(1)	105.66(1)	69.69(1)
γ/(°)	90	90	79.59(1)
Volume/nm³	5.484(1)	2.3482(5)	0.7101(2)
Z	4	4	1
ρ_calcd/(g·cm^-3)	1.594	1.705	1.437
Absorption coefficient/mm^-1	1.079	1.251	1.076
Obsd. data[I>2σ(I)]	1894	1601	6118
GOF	0.960	0.964	1.055
R₁[I>2σ(I)]	0.0916	0.0862	0.0477
wR₂(All data)	0.1663	0.1627	0.1356

Table 1 Crystallographic data for complexes 1—3

Compound	1	2	3·6CH₃CN
Empirical formula	C₃₆H₅₆ $N 2 0$ O₁₆Cl₂Mn₄	C₃₀ $H 4 6$ N₁₈O₁₆Cl₂Mn₄	$C 4 2$ H₆₀N₁₈O₆Cl₄Mn₄
Formula weight	1315.67	1205.51	1274.64
Crystal system	Monoclinic	Monoclinic	Triclinic
Space group	C2/c	P2₁/c	P-1
a/nm	2.8773(4)	1.2276(2)	1.0440(3)
b/nm	1.8427(2)	1.0738(2)	1.1281(4)
c/nm	1.0991(2)	1.8502(2)	1.3646(3)
α/(°)	90	90	80.57(1)
β/(°)	109.77(1)	105.66(1)	69.69(1)
γ/(°)	90	90	79.59(1)
Volume/nm³	5.484(1)	2.3482(5)	0.7101(2)
Z	4	4	1
ρ_calcd/(g·cm^-3)	1.594	1.705	1.437
Absorption coefficient/mm^-1	1.079	1.251	1.076
Obsd. data[I>2σ(I)]	1894	1601	6118
GOF	0.960	0.964	1.055
R₁[I>2σ(I)]	0.0916	0.0862	0.0477
wR₂(All data)	0.1663	0.1627	0.1356

Fig.1 Crystal structure of the tetranuclear complex 1

Fig.2 Crystal structure of the tetranuclear complex 2

Fig.3 Crystal structure of the tetranuclear complex 3·6CH3CN(A) and 1D supramolecular chain via π…π contacts(dotted lines)(B)

Table 2 Selected bond distances(nm) and bond angles(°) for complexe 1

Mn1—O1A	0.1903(6)	Mn1—O2	0.1971(6)
Mn1—O3	0.1883(6)	Mn1—O4	0.2179(7)
Mn1—O2A	0.2230(6)	Mn1—N8	0.1986(7)
Mn2—O1	0.2182(6)	Mn2—O2	0.2406(6)
Mn2—O3	0.2164(6)	Mn2—N1	0.2199(9)
Mn2—N3	0.2131(9)	Mn2—N5	0.2168(8)
Mn1—O2—Mn2	98.9(2)	Mn1—O3—Mn2	110.9(3)
Mn1A—O1—Mn2	110.1(3)	Mn1A—O2—Mn2	92.5(2)
Mn1—O2—Mn1A	103.4(3)

Table 3 Selected bond distances(nm) and bond angles(°) for complexe 2

Mn1—O1	0.1907(5)	Mn1—O2	0.1939(5)
Mn1—O2A	0.2326(5)	Mn1—O3A	0.1874(5)
Mn1—N1	0.1981(9)	Mn1—N7	0.2174(8)
Mn2—O1	0.2131(6)	Mn2—O2	0.2344(5)
Mn2—O3	0.2215(6)	Mn2—O1W	0.2260(6)
Mn2—N3	0.2168(9)	Mn2—N5	0.2160(8)
Mn1—O1—Mn2	108.1(3)	Mn1—O2—Mn2	99.2(2)
Mn1A—O2—Mn2	94.5(2)	Mn1A—O3—Mn2	113.7(3)
Mn1—O2—Mn1A	101.3(2)

Table 4 Selected bond distances(nm) and bond angles(°) for complexe 3·6CH3CN

Mn1—O1	0.1871(2)	Mn1—O2	0.1906(2)
Mn1—O3	0.2353(2)	Mn1—O3A	0.1930(2)
Mn1—N3	0.2021(2)	Mn1—Cl1	0.2509(1)
Mn2—O1	0.2296(2)	Mn2—O2A	0.2139(2)
Mn2—O3	0.2380(2)	Mn2—N1	0.2160(2)
Mn2—N5	0.2177(2)	Mn2—Cl2	0.2466(1)
Mn1—O1—Mn2	113.23(9)	Mn1—O3—Mn2	94.95(6)
Mn1—O2—Mn2A	108.66(8)	Mn1A—O3—Mn2	98.99(8)
Mn1—O3—Mn1A	101.56(7)

Fig.4 Temperature dependence of χmT for complex 1The solid line represents the best fit results(2—300 K) using the parameters discussed in the text.

Fig.5 Temperature dependence of χmT for complex 2The solid line represents the best fit results(20—300 K) using the parameters discussed in the text.

Fig.6 Temperature dependence of χmT for complex 3·6H2OThe solid line represents the best fit results(5—300 K) using the parameters discussed in the text.

Fig.7 Magnetic coupling in Mn4 complexes 1—3

Table 5 Comparison of the magnetic property for butterfly Mn4 complexes

Compound	(J_bb/k_B)/ K	Mn^Ⅲ—O—Mn^Ⅲ/ (°)	(J_wb/k_B)/ K	Mn^Ⅲ—O—Mn^Ⅱ/ (°)	$θ avg *$ / (°)	Ref.
[Mn₄(hmmi)₆Cl₄](3)	14.4	101.56	-1.35	94.95, 98.99, 108.66, 113.23	104.0	This work
[Mn₄(hmp)₆(Hhmp)₂](ClO₄)₄	0.25	102.90	-0.92	94.35, 97.24, 105.36, 110.59	101.9	[17]
[Mn₄(hmp)₄(acac)₂(MeO)₂](ClO₄)₂	2.7	99.38	0.39	96.84, 107.19	102.0	[21]
[Mn₄(hmp)₆(NO₃)₂(MeCN)₂](ClO₄)₂	5.0	99.55	0.5	95.33, 99.77, 107.76, 109.34	103.1	[21]
[Mn₄(hmp)₆(H₂O)₄](ClO₄)₄	5.0	98.9	0.55	93.8, 100.0, 106.6, 111.8	103.1	[17]
[Mn₄(hmmi)₆(DMF)₂(N₃)₂](ClO₄)₂(1)	4.5	103.4	0.63	92.5, 98.9, 110.1, 110.9	103.1	This work
[Mn₄(hmp)₆(CH₃CN)₂(H₂O)₄](ClO₄)₄	8.56	100.49	0.66	94.41, 99.84, 107.64, 113.28	103.8	[17]
[Mn₄(hmp)₆(H₂O)₂(NO₃)₂](NO₃)₂	7.1	98.81	0.80	95.00, 100.43, 107.53, 111.68	103.7	[16]
{[Mn₄(hmp)₆(NO₃)₂][FeNO(CN)₅]}_n	9.78	99.01	0.91	94.09, 99.83, 107.73, 110.36	103.0	[25]
[Mn₄(hmp)₆(dca)₂](ClO₄)₂	9.12	98.19, 98.61	1.02	95.42, 99.73, 106.25, 109.12	102.6	[18]
[Mn₄(hmp)₄(Hpdm)₂(dca)₂](ClO₄)₂	12.66	100.60	1.15	94.67, 100.78, 109.06, 111.05	102.4	[18]
[Mn₄(hmp)₆(H₂O)₂(NO₃)₂](ClO₄)₂	13.3	99.44	1.24	95.31, 100.25, 107.63, 110.77	103.5	[17]
[Mn₄(hmp)₆(dae-c)₂(H₂O)₂](ClO₄)₂	12.26	100.51	1.25	94.07, 99.91, 107.75, 109.19	102.7	[19]
[Mn₄(hmp)₆(dae-o)₂(ClO₄)₂]	9.18	99.44	1.26	96.70, 109.70	103.2	[19]
[Mn₄(hmp)₄Br₂(OMe)₂(dca)₂]	10.89	97.71	1.30	97.23, 98.40, 109.10, 109.69	103.6	[18]
[Mn₄(hmp)₆(NO₃)₂(dca)₂]	9.80	98.91	1.61	95.49, 101.14, 108.06, 109.84	103.6	[18]
[Mn₄(hmp)₆(NO₃)₄]	3.2	99.03	2.1	96.89, 99.47, 107.42, 110.67	103.6	[21]
[Mn₄(hmp)₆(N₃)₄]	3.96	100.48	2.78	94.70, 111.73, 97.81, 108.23	103.1	[28]
[Mn₄(hmmi)₆(H₂O)₂(N₃)₂](ClO₄)₂(2)	13.7	101.3	2.37	94.5, 99.2, 108.1, 113.7	103.9	This work

Table 5 Comparison of the magnetic property for butterfly Mn4 complexes

Compound	(J_bb/k_B)/ K	Mn^Ⅲ—O—Mn^Ⅲ/ (°)	(J_wb/k_B)/ K	Mn^Ⅲ—O—Mn^Ⅱ/ (°)	$θ avg *$ / (°)	Ref.
[Mn₄(hmmi)₆Cl₄](3)	14.4	101.56	-1.35	94.95, 98.99, 108.66, 113.23	104.0	This work
[Mn₄(hmp)₆(Hhmp)₂](ClO₄)₄	0.25	102.90	-0.92	94.35, 97.24, 105.36, 110.59	101.9	[17]
[Mn₄(hmp)₄(acac)₂(MeO)₂](ClO₄)₂	2.7	99.38	0.39	96.84, 107.19	102.0	[21]
[Mn₄(hmp)₆(NO₃)₂(MeCN)₂](ClO₄)₂	5.0	99.55	0.5	95.33, 99.77, 107.76, 109.34	103.1	[21]
[Mn₄(hmp)₆(H₂O)₄](ClO₄)₄	5.0	98.9	0.55	93.8, 100.0, 106.6, 111.8	103.1	[17]
[Mn₄(hmmi)₆(DMF)₂(N₃)₂](ClO₄)₂(1)	4.5	103.4	0.63	92.5, 98.9, 110.1, 110.9	103.1	This work
[Mn₄(hmp)₆(CH₃CN)₂(H₂O)₄](ClO₄)₄	8.56	100.49	0.66	94.41, 99.84, 107.64, 113.28	103.8	[17]
[Mn₄(hmp)₆(H₂O)₂(NO₃)₂](NO₃)₂	7.1	98.81	0.80	95.00, 100.43, 107.53, 111.68	103.7	[16]
{[Mn₄(hmp)₆(NO₃)₂][FeNO(CN)₅]}_n	9.78	99.01	0.91	94.09, 99.83, 107.73, 110.36	103.0	[25]
[Mn₄(hmp)₆(dca)₂](ClO₄)₂	9.12	98.19, 98.61	1.02	95.42, 99.73, 106.25, 109.12	102.6	[18]
[Mn₄(hmp)₄(Hpdm)₂(dca)₂](ClO₄)₂	12.66	100.60	1.15	94.67, 100.78, 109.06, 111.05	102.4	[18]
[Mn₄(hmp)₆(H₂O)₂(NO₃)₂](ClO₄)₂	13.3	99.44	1.24	95.31, 100.25, 107.63, 110.77	103.5	[17]
[Mn₄(hmp)₆(dae-c)₂(H₂O)₂](ClO₄)₂	12.26	100.51	1.25	94.07, 99.91, 107.75, 109.19	102.7	[19]
[Mn₄(hmp)₆(dae-o)₂(ClO₄)₂]	9.18	99.44	1.26	96.70, 109.70	103.2	[19]
[Mn₄(hmp)₄Br₂(OMe)₂(dca)₂]	10.89	97.71	1.30	97.23, 98.40, 109.10, 109.69	103.6	[18]
[Mn₄(hmp)₆(NO₃)₂(dca)₂]	9.80	98.91	1.61	95.49, 101.14, 108.06, 109.84	103.6	[18]
[Mn₄(hmp)₆(NO₃)₄]	3.2	99.03	2.1	96.89, 99.47, 107.42, 110.67	103.6	[21]
[Mn₄(hmp)₆(N₃)₄]	3.96	100.48	2.78	94.70, 111.73, 97.81, 108.23	103.1	[28]
[Mn₄(hmmi)₆(H₂O)₂(N₃)₂](ClO₄)₂(2)	13.7	101.3	2.37	94.5, 99.2, 108.1, 113.7	103.9	This work

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Synthesis, Crystal Structure and Magnetic Properties of Tetranuclear Mn^Ⅱ₂Mn^Ⅲ₂ Complexes Based on 2-(Hydroxymethyl)-N-methylimidazole^†

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