crystal structure of dichlorobis 2 pyridinealdoxime n n manganese ii dihydrate mncl2 c6h6n2o 2 2h2o

Z Kristallogr NCS 225 (2010) 651-652 / DOI 10.1524/ncrs.2010.0284 651 © by Oldenbourg Wissenschaftsverlag, München Crystal structure of dichlorobis(2-pyridinealdoxime-N,N')manganese(II) dihydrate, MnCl2(C6H6N2O)2 · 2H2O Kwang Ha* Chonnam National University, School of Applied Chemical Engineering, Research Institute of Catalysis, Gwangju 500-757, Republic of Korea Received July 13, 2010, accepted and available on-line September 27, 2010; CCDC no 1267/3156 are nearly equivalent with d(Mn—Npyridine) = 2.322(2) Å and 2.260(2) Å and d(Mn—Noxime) = 2.322(2) Å and 2.342(2) Å The complex displays intermolecular p-p interactions between adjacent pyridine rings For Cg1 (the centroid of ring N3-C11) and Cg1i (symmetry code i: –x,1–y,–z), the centroid-centroid distance is 3.993(2) Å, the planes are parallel and shifted for 1.880 Å All H atoms on the O atoms participate in intermolecular O–H···O or O–H···Cl hydrogen bonds with d(O···O) = 2.605(3) - 2.816(4) Å and d(O···Cl) = 3.017(3) - 3.213(3) Å Table Data collection and handling Abstract C12H16Cl2MnN4O4, monoclinic, P121/c1 (no 14), a = 14.6283(7) Å, b = 13.9519(6) Å, c = 8.7216(4) Å, b = 101.565(1)°, V = 1743.9 Å3, Z = 4, Rgt(F) = 0.039, wRref(F2) = 0.108, T = 200 K Source of material To a solution of MnCl2 · 4H2O (1.00 g, 5.05 mmol) in H2O (5 ml) was added syn-2-pyridinealdoxime (1.86 g, 15.23 mmol) in EtOH (55 ml) and stirred for h at room temparature The solvent was removed under vacuum, the residue was washed with ether, and dried, to give a pale yellow powder (1.79 g) Crystals suitable for X-ray diffraction analysis were obtained by slow evaporation from a CH3CN solution Experimental details Hydrogen atoms were positioned geometrically and allowed to ride on their parent atoms with d(C—H) = 0.95 Å, d(O—H) = 0.84 Å and Uiso(H) = 1.2 Ueq(C) or 1.5 Ueq(O) Discussion The crystal structure of the title compound consists of the neutral complex [MnCl2(C6H6N2O)2] and two uncoordinated water molecules In the complex, the central Mn(II) ion has a distorted octahedral coordination defined by four N atoms of the two chelating 2-pyridinealdoxime ligands and two Cl anions The main contribution to the distortion is the tight N–Mn–N chelate angles (71.13(9)° and 71.59(8)°), which results in non-linear trans axes (∠Cl1–Mn1–N1 = 165.83(6)°, ∠Cl2–Mn1–N4 = 168.56(6)° and ∠N2–Mn1–N3 = 160.88(8)°) Moreover, the Cl-Cl repelling is present (∠Cl1–Mn1–Cl2 = 96.99(3)°), which also contributes to the distortion The bond lengths Mn—Npyridine and Mn—Noxime Crystal: Wavelength: m: Diffractometer, scan mode: 2qmax: N(hkl)measured, N(hkl)unique: Criterion for Iobs, N(hkl)gt: N(param)refined: Programs: yellow block, size 0.24 × 0.31 × 0.38 mm Mo Ka radiation (0.71073 Å) 10.85 cm−1 Bruker SMART 1000 CCD, j/w 56.58° 12494, 4288 Iobs > s(Iobs), 3184 210 SHELXS-97, SHELXL-97 [1], ORTEP [2], PLATON [3] Table Atomic coordinates and displacement parameters (in Å2) Atom Site H(1A) H(2A) H(1) H(2) H(3) H(4) H(6) H(7) H(8) H(9) H(10) H(12) H(3A) H(3B) H(4A) H(4B) 4e 4e 4e 4e 4e 4e 4e 4e 4e 4e 4e 4e 4e 4e 4e 4e x 0.3839 0.1753 0.2314 0.3129 0.4526 0.5077 0.4900 0.1646 0.0305 −0.0916 −0.0758 0.0185 0.7303 0.7159 0.6939 0.7443 _ * e-mail: hakwang@chonnam.ac.kr Brought to you by | HEC Bibliotheque Maryriam ET J Authenticated Download Date | 7/17/15 1:06 PM y 0.6428 0.4880 0.2575 0.1169 0.1233 0.2721 0.4493 0.4357 0.3748 0.3212 0.3285 0.3755 0.1294 0.0715 0.2084 0.2734 z 0.6305 0.7253 0.3041 0.3771 0.5614 0.6611 0.6690 0.0142 −0.1458 −0.0316 0.2404 0.5030 0.7064 0.5861 0.3249 0.4269 Uiso 0.082 0.081 0.052 0.064 0.069 0.061 0.047 0.043 0.048 0.051 0.047 0.044 0.098 0.098 0.103 0.103 652 MnCl2(C6H6N2O)2 · 2H2O Table Atomic coordinates and displacement parameters (in Å2) Atom Site Mn(1) Cl(1) Cl(2) O(1) O(2) N(1) N(2) N(3) N(4) C(1) C(2) C(3) C(4) C(5) C(6) C(7) C(8) C(9) C(10) C(11) C(12) O(3) O(4) 4e 4e 4e 4e 4e 4e 4e 4e 4e 4e 4e 4e 4e 4e 4e 4e 4e 4e 4e 4e 4e 4e 4e x 0.24446(3) 0.16204(6) 0.33276(5) 0.4234(2) 0.1397(2) 0.3183(2) 0.3782(2) 0.1250(2) 0.1389(2) 0.2885(2) 0.3365(3) 0.4185(3) 0.4503(2) 0.3984(2) 0.4303(2) 0.1149(2) 0.0353(2) −0.0362(2) −0.0271(2) 0.0539(2) 0.0653(2) 0.7487(2) 0.7008(2) y z 0.49322(3) 0.64502(6) 0.53913(5) 0.5991(2) 0.4434(2) 0.3465(2) 0.5160(2) 0.4199(2) 0.4374(2) 0.2607(2) 0.1763(2) 0.1801(3) 0.2675(3) 0.3492(2) 0.4428(2) 0.4140(2) 0.3777(2) 0.3461(2) 0.3507(2) 0.3882(2) 0.3981(2) 0.0768(2) 0.2666(2) 0.37807(5) 0.3842(1) 0.17676(8) 0.6301(3) 0.6859(2) 0.4359(3) 0.5688(3) 0.2159(3) 0.5271(3) 0.3784(4) 0.4213(4) 0.5286(5) 0.5878(4) 0.5403(3) 0.6028(3) 0.0608(3) −0.0357(3) 0.0316(4) 0.1918(4) 0.2807(3) 0.4507(3) 0.6766(3) 0.3486(3) U11 U22 U33 0.0266(2) 0.0489(4) 0.0353(4) 0.043(1) 0.066(2) 0.030(1) 0.033(1) 0.028(1) 0.041(1) 0.042(2) 0.062(2) 0.055(2) 0.042(2) 0.034(2) 0.025(1) 0.035(2) 0.046(2) 0.039(2) 0.036(2) 0.028(1) 0.039(2) 0.078(2) 0.079(2) 0.0310(2) 0.0382(4) 0.0462(4) 0.046(1) 0.073(2) 0.035(1) 0.037(1) 0.033(1) 0.039(1) 0.035(2) 0.032(2) 0.040(2) 0.052(2) 0.039(2) 0.051(2) 0.041(2) 0.045(2) 0.045(2) 0.039(2) 0.029(1) 0.039(2) 0.078(2) 0.048(2) 0.0289(2) 0.0492(5) 0.0337(4) 0.071(2) 0.024(1) 0.036(1) 0.035(1) 0.027(1) 0.028(1) 0.051(2) 0.067(2) 0.079(3) 0.056(2) 0.036(2) 0.038(2) 0.032(2) 0.028(1) 0.039(2) 0.044(2) 0.035(1) 0.035(2) 0.033(1) 0.072(2) Acknowledgment This work was supported by Priority Research Centers Program through the National Research Foundation of Korea (NRF) funded by the Ministry of Education, Science and Technology (grant no 20090094056) References Sheldrick, G M.: A short history of SHELX Acta Crystallogr A64 (2008) 112-122 Farrugia, L J.: ORTEP-3 for Windows - a version of ORTEP-III with a Graphical User Interface (GUI) J Appl Crystallogr 30 (1997) 565 Spek, A L.: Single-crystal structure validation with the program PLATON J Appl Crystallogr 36 (2003) 7-13 Brought to you by | HEC Bibliotheque Maryriam ET J Authenticated Download Date | 7/17/15 1:06 PM U12 −0.0009(2) 0.0108(3) −0.0046(3) −0.008(1) −0.019(1) 0.002(1) −0.007(1) −0.0029(9) 0.000(1) −0.002(1) −0.001(2) 0.012(2) 0.010(2) 0.001(1) 0.001(1) −0.006(1) −0.009(1) −0.013(1) −0.010(1) −0.002(1) −0.005(1) 0.024(2) 0.011(1) U13 0.0017(2) 0.0040(4) 0.0057(3) 0.000(1) 0.012(1) 0.007(1) 0.005(1) 0.0032(9) 0.010(1) 0.004(2) 0.018(2) 0.015(2) 0.000(2) 0.009(1) −0.006(1) 0.007(1) 0.003(1) −0.002(1) 0.011(1) 0.006(1) 0.015(1) −0.002(1) −0.004(2) U23 −0.0005(2) −0.0018(3) 0.0036(3) −0.018(1) −0.004(1) 0.004(1) −0.005(1) −0.0008(9) −0.001(1) −0.002(1) 0.005(2) 0.017(2) 0.014(2) 0.009(1) 0.003(1) −0.001(1) −0.003(1) −0.002(1) 0.001(1) 0.001(1) 0.000(1) −0.001(1) −0.014(1) ...6 52 MnCl2( C6H 6N2 O )2 · 2H2O Table Atomic coordinates and displacement parameters (in ? ?2) Atom Site Mn(1) Cl(1) Cl (2) O(1) O (2) N( 1) N (2) N( 3) N( 4) C(1) C (2) C(3) C(4) C(5) C(6)... 0.4503 (2) 0.3984 (2) 0.4303 (2) 0.1149 (2) 0.0353 (2) −0.03 62( 2) −0. 027 1 (2) 0.0539 (2) 0.0653 (2) 0.7487 (2) 0.7008 (2) y z 0.49 322 (3) 0.645 02( 6) 0.53913(5) 0.5991 (2) 0.4434 (2) 0.3465 (2) 0.5160 (2) 0.4199 (2) ... 0.4199 (2) 0.4374 (2) 0 .26 07 (2) 0.1763 (2) 0.1801(3) 0 .26 75(3) 0.34 92( 2) 0.4 428 (2) 0.4140 (2) 0.3777 (2) 0.3461 (2) 0.3507 (2) 0.38 82( 2) 0.3981 (2) 0.0768 (2) 0 .26 66 (2) 0.37807(5) 0.38 42( 1) 0.17676(8)