158
Z. Kristallogr. NCS 227 (2012) 158-160 / DOI 10.1524/ncrs.2012.0071
© by Oldenbourg Wissenschaftsverlag, München
Crystal structure of bis(2,2'-bipyridyl)-hexa[--2-(4'-chlorobenzoyl)benzoato-"2O:O')trimanganese(II), Mn3(C10H8N2)2(C14H8O3Cl)6 Xiu-Mei Li*,I, Bo LiuII and Qing-Wei WangII I II
Department of Chemistry, Tonghua Teachers College, Tonghua 134002, Jilin, P. R. China Department of Chemistry, Jilin Normal University, Siping 136000, Jilin, P. R. China
Received October 9, 2011, accepted and available on-line February 27, 2012; CCDC no. 1267/3708
Abstract C104H64Cl6Mn3N4O18, triclinic, P1 (no. 2), a = 12.331(3) Å, b = 14.065(3) Å, c = 14.803(3) Å, * = 86.552(4)°, ) = 69.715(3)°, ' = 73.444(4)°, V = 2306.1 Å3, Z = 1, Rgt(F) = 0.043, wRref(F2) = 0.109, T = 292 K. Source of material A mixture of Mn(CH3COO)2) , 4H2O (0.2 mmol, 0.05 g), 2-(4'chlorobenzoyl)benzoic acid (0.4 mmol, 0.10 g), 2,2'-bipyridine (0.2 mmol, 0.032 g) and H2O (18 mL) was placed in a 30 mL Teflon-lined autoclave under autogenous pressure at 423 K for seven days. After cooling to room temperature, yellow block-shaped crystals were collected by filtration and washed with distilled water in 42 % yield (based on Mn). Elemental analysis — found: C, 61.2 %; H, 3.14 %; N, 2.5 %; calculated for C104H64Cl6Mn3N4O18: C, 61.4 %; H, 3.17 %; N, 2.8 %. Discussion Recently, the design and synthesis of coordination compounds have attracted much attention due to their structural diversity [12] and potential applications [2-8]. A successful strategy for preparing coordination compounds is the assembly reaction between _____________
* Correspondence author (e-mail:
[email protected])
a transition metal ion and two types of organic molecules, one acting as a terminal ligand and the other as a bridging ligand. In this aspect, the rigid and versatile ligand 2-(4'-chlorobenzoyl)benzoic acid (Hcbba) has been relatively less studied for constructing coordination compounds containing transition metals [9-10]. In the title crystal structure, the asymmetric unit contains one and a half Mn(II) atoms, three 2-(4'-chlorobenzoyl)benzoate (cbba) ligands and one 2,2'-bipyridine ligand. The Mn1 atom is six-coordinated by six carboxylate oxygen atoms (O1, O4, O5, O1A, O4A, O5A) from six different cbba ligands, forming a slightly distorted octahedron (d(Mn1—O1) = 2.124(2) Å, d(Mn1—O4) = 2.192(2) Å, d(Mn1—O5) = 2.140(2) Å, d(Mn1—O1A) = 2.124(2) Å, d(Mn1—O4A) = 2.192(2) Å, d(Mn1—O5A) = 2.140(2) Å). The Mn2 atom is five-coordinated by three carboxylate oxygen atoms (O2, O3, O6) from three different cbba ligands and two nitrogen atoms (N1, N2) from 2,2'-bipyridine ligand, forming a distorted square pyramid (d(Mn2—O2) = 2.112(2) Å, d(Mn2—O3) = 2.182(2) Å, d(Mn2—O6) = 2.270(2) Å, d(Mn2—N1) = 2.267(2) Å, d(Mn2—N2) = 2.299(2) Å). The angles N(O)–Mn–O(N) range from 53.81(7)° to 180.0(1)°. The cbba ligand presents only bidentate bridging mode in the title crystal structure. As a result, the carboxyl oxygen atoms link the Mn atoms to form a trinuclear compound.
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Mn3(C10H8N2)2(C14H8O3Cl)6
159 Table 2. Continued.
Table 1. Data collection and handling. Crystal: Wavelength: -: Diffractometer, scan mode: 2+max: N(hkl)measured, N(hkl)unique: Criterion for Iobs, N(hkl)gt: N(param)refined: Programs:
yellow block, size 0.156 " 0.170 " 0.369 mm Mo K* radiation (0.71073 Å) 6.52 cm&1 Bruker APEXII CCD, #/& 52.02° 12703, 8940 Iobs > 2 ((Iobs), 6108 610 SHELXS-97, SHELXL-97, SHELXTL [11]
Table 2. Atomic coordinates and displacement parameters (in Å2). Atom
Site
x
y
H(13A) H(16A) H(17A) H(27A) H(38A) H(18A) H(30A)
2i 2i 2i 2i 2i 2i 2i
0.8956 1.3665 1.3200 0.8347 1.2037 1.1349 1.1747
0.4532 0.3013 0.4626 0.2780 &0.0381 0.5340 0.1290
z
Uiso
0.9231 0.3994 0.4547 0.3327 0.1673 0.5708 0.0776
0.092 0.096 0.104 0.056 0.068 0.083 0.079
Atom
Site
x
y
H(7A) H(3A) H(10A) H(28A) H(14A) H(24A) H(15A) H(35A) H(34A) H(22A) H(11A) H(29A) H(5A) H(21A) H(6A) H(41A) H(23A) H(48A) H(4A) H(52A) H(49A) H(44A) H(51A) H(42A) H(43A)
2i 2i 2i 2i 2i 2i 2i 2i 2i 2i 2i 2i 2i 2i 2i 2i 2i 2i 2i 2i 2i 2i 2i 2i 2i
1.3454 1.2924 1.2190 0.8247 0.8670 0.7229 1.2276 1.6113 1.4721 0.7703 1.2478 0.9960 1.3257 0.9610 1.1567 0.7151 0.6512 0.5018 1.3994 0.4653 0.4361 0.3785 0.3964 0.5479 0.3798
&0.1776 &0.1061 0.1816 0.2724 0.2976 0.3817 0.2140 &0.0724 0.0657 0.6452 0.3365 0.2001 &0.1246 0.5904 0.0071 0.0006 0.5367 0.3040 &0.1776 0.5257 0.4179 0.2489 0.6388 &0.0394 0.0835
z
Uiso
0.0788 0.6254 0.7877 0.1804 0.9218 0.7633 0.4603 0.0852 0.1739 0.7911 0.7895 0.0526 0.8857 0.6768 0.9434 0.6096 0.8379 0.7835 0.7258 0.6040 0.9104 0.6067 0.7302 0.6092 0.6078
0.081 0.066 0.086 0.070 0.077 0.073 0.075 0.078 0.068 0.095 0.103 0.083 0.096 0.076 0.082 0.061 0.091 0.070 0.084 0.078 0.083 0.084 0.092 0.086 0.097
Table 3. Atomic coordinates and displacement parameters (in Å2). Atom
Site
x
Mn(1) Mn(2) Cl(2) Cl(1) O(2) O(5) C(13) O(6) O(1) O(3) C(16) C(17) O(4) O(8) O(7) N(2) N(1) C(27) C(26) C(9) C(19) C(31) C(38) C(18) C(30) C(33) C(25) C(7) C(37) C(2) C(1) C(3) C(20) C(10) C(32) C(8) C(12) C(28) C(14)
1b 2i 2i 2i 2i 2i 2i 2i 2i 2i 2i 2i 2i 2i 2i 2i 2i 2i 2i 2i 2i 2i 2i 2i 2i 2i 2i 2i 2i 2i 2i 2i 2i 2i 2i 2i 2i 2i 2i
1 0.94835(4) 1.5969(1) 1.0942(1) 1.0426(2) 0.8539(2) 0.9607(4) 0.7486(2) 1.1050(2) 0.9454(2) 1.2923(3) 1.2645(4) 1.0626(2) 1.2671(2) 0.9185(2) 1.1008(2) 0.8815(2) 0.9035(3) 1.0107(2) 1.0398(3) 1.0735(3) 1.1146(3) 1.2855(3) 1.1546(3) 1.1063(3) 1.3228(3) 1.0072(3) 1.1254(3) 1.3702(4) 1.1659(3) 1.0989(2) 1.2664(3) 0.9522(3) 1.1532(3) 1.2364(3) 1.0187(3) 1.0740(4) 0.8976(3) 0.9443(3)
y 0 0.24329(3) &0.23651(7) 0.52500(8) 0.1378(1) 0.1073(2) 0.3982(3) 0.2610(1) &0.0076(1) 0.2803(2) 0.3307(3) 0.4263(3) 0.1263(2) 0.1734(2) 0.1131(2) 0.3187(2) 0.3910(2) 0.2473(2) 0.2046(2) 0.2227(2) 0.4127(2) 0.1596(2) &0.0441(2) 0.4690(3) 0.1588(2) 0.0305(2) 0.2038(2) 0.0358(2) &0.1276(2) &0.0002(2) 0.0474(2) &0.0812(2) 0.4528(2) 0.2360(2) 0.1238(2) 0.1235(2) 0.4076(3) 0.2446(2) 0.3049(3)
z ½ 0.59714(3) &0.00042(8) 0.8540(1) 0.6712(1) 0.5998(1) 0.8957(3) 0.6353(2) 0.5890(1) 0.4526(1) 0.4460(3) 0.4790(3) 0.4313(2) 0.2775(2) 0.8972(2) 0.5505(2) 0.6803(2) 0.2815(2) 0.2978(2) 0.8549(2) 0.5827(2) 0.2208(2) 0.1499(2) 0.5479(3) 0.1295(2) 0.1769(2) 0.4005(2) 0.8168(2) 0.0970(2) 0.7210(2) 0.6547(2) 0.6884(2) 0.6557(2) 0.8153(2) 0.2308(2) 0.8572(2) 0.8557(3) 0.1903(2) 0.8948(2)
U11
U22
U33
0.0402(3) 0.0423(3) 0.1135(9) 0.181(1) 0.073(2) 0.044(1) 0.092(3) 0.050(1) 0.058(1) 0.061(1) 0.052(2) 0.067(3) 0.073(2) 0.062(2) 0.071(2) 0.050(2) 0.045(2) 0.052(2) 0.051(2) 0.058(2) 0.055(2) 0.054(2) 0.057(2) 0.070(3) 0.068(2) 0.050(2) 0.049(2) 0.065(2) 0.090(3) 0.054(2) 0.044(2) 0.059(2) 0.057(2) 0.064(2) 0.052(2) 0.067(2) 0.101(3) 0.066(2) 0.065(2)
0.0245(3) 0.0290(2) 0.0560(6) 0.0699(7) 0.037(1) 0.071(1) 0.062(2) 0.049(1) 0.047(1) 0.061(1) 0.110(3) 0.109(3) 0.056(1) 0.061(1) 0.093(2) 0.049(1) 0.041(1) 0.042(2) 0.031(1) 0.059(2) 0.045(2) 0.044(2) 0.054(2) 0.065(2) 0.078(2) 0.049(2) 0.041(2) 0.051(2) 0.047(2) 0.041(2) 0.037(2) 0.040(2) 0.036(2) 0.063(2) 0.047(2) 0.072(2) 0.063(2) 0.056(2) 0.075(2)
0.0327(3) 0.0385(2) 0.0927(7) 0.166(1) 0.055(1) 0.058(1) 0.071(2) 0.073(1) 0.046(1) 0.041(1) 0.074(2) 0.100(3) 0.071(1) 0.066(1) 0.075(2) 0.045(1) 0.049(1) 0.047(2) 0.041(2) 0.037(2) 0.050(2) 0.043(2) 0.060(2) 0.085(3) 0.045(2) 0.041(2) 0.044(2) 0.047(2) 0.065(2) 0.048(2) 0.039(2) 0.077(2) 0.052(2) 0.085(2) 0.043(2) 0.036(2) 0.076(3) 0.060(2) 0.054(2)
U12 &0.0054(2) &0.0088(2) &0.0012(5) &0.0609(8) &0.011(1) 0.008(1) &0.008(2) &0.017(1) &0.0059(9) &0.016(1) &0.032(2) &0.054(3) &0.033(1) &0.017(1) &0.047(2) &0.015(1) &0.014(1) &0.012(1) &0.016(1) &0.025(2) &0.020(1) &0.012(1) &0.017(2) &0.036(2) &0.006(2) &0.014(1) &0.024(1) &0.032(2) &0.022(2) &0.023(1) &0.016(1) &0.018(2) &0.015(1) &0.029(2) &0.018(1) &0.037(2) &0.035(2) &0.011(2) &0.023(2)
U13 &0.0144(2) &0.0151(2) 0.0141(6) &0.078(1) &0.039(1) &0.020(1) &0.032(2) &0.016(1) &0.027(1) &0.018(1) &0.007(2) &0.027(2) &0.044(1) &0.026(1) &0.014(1) &0.018(1) &0.014(1) &0.019(1) &0.022(1) &0.017(1) &0.028(2) &0.021(1) &0.019(2) &0.031(2) &0.021(2) &0.014(1) &0.019(1) &0.032(2) &0.022(2) &0.029(1) &0.018(1) &0.037(2) &0.028(2) &0.010(2) &0.014(1) &0.023(2) &0.034(2) &0.036(2) &0.020(2)
U23 &0.0012(2) &0.0003(2) &0.0023(5) 0.0017(7) 0.0034(9) &0.022(1) &0.005(2) &0.012(1) &0.0049(9) &0.006(1) &0.001(2) 0.026(3) 0.033(1) &0.010(1) 0.004(1) 0.000(1) &0.004(1) 0.003(1) 0.006(1) &0.001(1) 0.012(1) 0.000(1) 0.000(2) 0.014(2) &0.006(2) 0.003(1) 0.010(1) 0.017(1) 0.002(2) 0.013(1) 0.005(1) 0.011(2) 0.005(1) &0.019(2) 0.003(1) 0.007(1) &0.003(2) 0.007(2) 0.002(2)
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160
Mn3(C10H8N2)2(C14H8O3Cl)6
Table 3. Continued. Atom
Site
x
C(24.) C(15) C(35) C(36) C(34) C(22) C(11) C(29) C(5) C(21) C(6) O(9) C(40) C(39) C(45) C(41) C(47) C(46) C(23) C(48) C(4) C(52) C(49) C(44) C(51) C(42) C(50) C(43) Cl(3)
2i 2i 2i 2i 2i 2i 2i 2i 2i 2i 2i 2i 2i 2i 2i 2i 2i 2i 2i 2i 2i 2i 2i 2i 2i 2i 2i 2i 2i
0.7720(3) 1.2088(3) 1.5293(3) 1.4905(3) 1.4461(3) 0.7984(4) 1.1709(4) 0.9994(3) 1.2859(4) 0.9117(3) 1.1854(4) 0.5792(3) 0.6487(2) 0.7568(2) 0.5483(3) 0.6471(3) 0.4944(3) 0.5458(3) 0.7273(3) 0.4824(3) 1.3290(3) 0.4602(3) 0.4426(3) 0.4467(3) 0.4195(3) 0.5476(4) 0.4127(3) 0.4475(4) 0.3675(1)
y 0.4240(2) 0.2790(3) &0.0648(3) &0.1359(2) 0.0177(2) 0.5811(2) 0.3284(3) 0.2010(3) &0.0928(3) 0.5484(2) &0.0138(3) 0.3602(2) 0.1491(2) 0.1740(2) 0.2240(2) 0.0509(2) 0.4020(2) 0.3311(2) 0.5173(3) 0.3715(2) &0.1259(2) 0.5036(2) 0.4391(2) 0.1992(3) 0.5712(2) 0.0268(3) 0.5387(2) 0.1000(3) 0.62475(8)
z
U11
U22
U33
U12
0.7463(2) 0.4829(2) 0.1010(2) 0.0718(2) 0.1535(2) 0.7638(3) 0.8159(3) 0.1143(2) 0.8444(3) 0.6958(2) 0.8789(3) 0.5129(2) 0.6104(2) 0.6147(2) 0.6073(2) 0.6096(2) 0.6790(2) 0.5944(2) 0.7909(3) 0.7723(2) 0.7492(3) 0.6655(3) 0.8485(2) 0.6073(2) 0.7404(3) 0.6090(2) 0.8312(3) 0.6080(3) 0.92619(9)
0.054(2) 0.049(2) 0.049(2) 0.068(2) 0.058(2) 0.092(3) 0.080(3) 0.081(3) 0.100(3) 0.081(3) 0.099(3) 0.121(2) 0.042(2) 0.039(2) 0.043(2) 0.061(2) 0.044(2) 0.054(2) 0.062(2) 0.060(2) 0.071(2) 0.049(2) 0.068(2) 0.045(2) 0.051(2) 0.085(3) 0.051(2) 0.069(3) 0.1044(9)
0.058(2) 0.076(2) 0.071(2) 0.047(2) 0.063(2) 0.045(2) 0.081(3) 0.083(2) 0.070(2) 0.035(2) 0.073(2) 0.068(2) 0.039(1) 0.051(2) 0.051(2) 0.046(2) 0.042(2) 0.052(2) 0.064(2) 0.045(2) 0.046(2) 0.049(2) 0.061(2) 0.091(3) 0.041(2) 0.069(2) 0.053(2) 0.109(3) 0.0798(7)
0.067(2) 0.061(2) 0.061(2) 0.051(2) 0.052(2) 0.095(3) 0.102(3) 0.045(2) 0.110(3) 0.074(2) 0.065(2) 0.056(2) 0.034(1) 0.031(1) 0.043(2) 0.044(2) 0.061(2) 0.054(2) 0.084(3) 0.058(2) 0.114(3) 0.078(2) 0.062(2) 0.074(2) 0.105(3) 0.067(2) 0.084(3) 0.082(3) 0.1217(9)
&0.016(2) &0.014(2) &0.009(2) &0.006(2) &0.020(2) &0.008(2) &0.046(2) &0.008(2) &0.039(2) &0.016(2) &0.043(2) &0.002(2) &0.011(1) &0.008(1) &0.013(1) &0.016(2) &0.005(1) &0.004(2) 0.000(2) &0.011(2) &0.020(2) &0.002(2) &0.011(2) &0.012(2) &0.001(2) &0.045(2) &0.008(2) &0.051(3) &0.0076(6)
U13 &0.012(2) &0.019(2) &0.009(2) &0.004(2) &0.018(2) &0.032(2) &0.014(2) &0.035(2) &0.079(3) &0.024(2) &0.054(2) &0.014(2) &0.013(1) &0.010(1) &0.017(1) &0.014(2) &0.013(2) &0.019(2) &0.011(2) &0.012(2) &0.056(2) &0.010(2) &0.008(2) &0.028(2) 0.002(2) &0.014(2) &0.001(2) &0.023(2) &0.0045(7)
U23 &0.015(2) &0.011(2) 0.007(2) 0.009(2) 0.003(2) &0.020(2) &0.016(2) &0.002(2) 0.041(2) &0.004(2) 0.023(2) 0.024(1) 0.004(1) &0.002(1) 0.006(1) 0.002(1) 0.013(1) 0.016(2) &0.036(2) 0.010(2) 0.021(2) 0.021(2) 0.001(2) 0.004(2) 0.006(2) &0.004(2) &0.012(2) &0.010(2) &0.0407(7)
Acknowledgment. This work was supported by Science and Technology Research Projects of China (grant no. 2011.459).
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7. Chen, B. L.; Eddaoudi, M.; Hyde, S. T.; O'Keeffe, M.; Yaghi, O. M.: Interwoven Metal-Organic Framework on a Periodic Minimal Surface with Extra-Large Pores. Science 291 (2001) 1021-1023. 8. Seo, J. S.; Whang, D.; Lee, H.; Jun, S. I.; Oh, J.; Jeon, Y. J.; Kim, K.: A homochiral metal-organic porous material for enantioselective separation and catalysis. Nature 404 (2000) 982-986. 9. Wang, Q. W.; Li, X. M.; Meng, Q. L.; Liu, B.; Gao, G. G.: Synthesis and Crystal Structure of a Manganese(II) Complex with 2-(4'-Chlorinebenzoyl)benzoic Acid and 1,10-Phenanthroline. Chinese J. Struct. Chem. 3 (2009) 335-337. 10. Li, X. M.; Wang, Q. W.; Liu, B.; Wang, Z. T.: Hydrothermal Synthesis and Crystal Structure of a Ni(II) Complex Assembled by 2-(4'-Chlorinebenzoyl)benzoic Acid and 1,10-Phenanthroline. Chinese J. Inorg. Chem. 10 (2010) 1904-1907. 11. Sheldrick, G. M.: A short history of SHELX. Acta Crystallogr. A64 (2008) 112-122.
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