J.-L. Ma

Crystal structure of bis(3,3′-diethyl-4-maleimidophenyl)methane, C25H22N2O4

Abstract C25H22N2O4, orthorhombic, Pccn (No. 56), a = 12.745(2) Å, b = 16.974(2) Å, c = 10.218(1) Å, V = 2210.4 Å3, Z = 4, Rgt(F) = 0.114, wRref(F2) = 0.300, T = 293 K.

Crystal structure of bis(2-aminopyrimidine)silver(I) hexafluoroarsenate bis(2-aminopyrimidine) solvate, [Ag(C4H5N3)2]AsF6 · 2C4H5N3

C 16 H 20 AgAsF 6 N 12 , triclinic, P1 (no. 2), a = 7.004(1) A, b = 8.696(2) A, c = 11.006(2) A, a = 68.95(3)°, β = 76.49(3)°, γ = 81.90(3)°, V = 607.1 A 3 , Z = 1, R gt (F) = 0.044, wR ref (F 2 ) = 0.111, T = 293 K.

Crystal structure of monoaquabenzoato-2,5,8-triaza-1,9-di(2-fluorobenzyl)-nonanecopper(II) benzoate dihydrate, Cu(C25H30F2N3O3)(C7H5O2).2H2O

C32H39C11F2N3O7, triclinio, P I (No. 2), a = 7.331(3) Â, b = 8.983(3) À, c = 26.34(1) À, a = 95.570(6)°, β = 95.797(6)°, γ = 110.811(5)°, V= 1596.3 À, Z = 2, Rgt(F) = 0.040, wRlei(F) = 0.103, T= 298 K. Source of material Dien and 2-fluorobenzaldehyde were condensed in anhydrous methanol and then reduced to obtain the ligand L, where dien is diethylenetriamine and L is 2,5,8-triaza-l,9-di(2-fluorobenzyl)nonane. Copper(II) benzoate (1.0 mmol, 306 mg) and L (1.0 mmol, 317 mg) were suspended in water (20 ml), stirring for ca. 1 hour to obtain a clear blue solution. After keeping the resulting solution in air for one week, large blue single crystals were formed on slow evaporation. The crystals were isolated, washed with water three times and dried in a vacuum desiccator using CaCl2 (yield 62%). Elemental analysis: found C, 56.08%; H, 5.90%; N, 6.11%; calc. forC32H39CuF2N307-C, 56.59%; H, 5.79; N, 6.19%. Experimental details All the H atoms were located from difference Fourier maps and refined isotropically. five-coordinated by three Ν atoms from an amine ligand, two O atoms from a benzoate ligand and a water molecule, respectively. N(l), N(2), N(3) and 0 ( 1 ) atoms constitute the basal plane (plane I) of the square-pyramid with the average deviation of 0.094 A, and Cu(l) atom locates 0.094  above I toward the axial 0(5) atom, which occupies the axial position. The average Cu—Ν bond length (2.023(4) Â) in the title complex is slightly shorter than those found in the similar copper(II) complex with the secondary amines (average d(Cu—N) = 2.10(3) Á [1], = 2.07(1) À [2]). The Cu(l)—0(1) distance of 1.958(2) À is much shorter than that 2.259(3)A found in the copper(II) complex with the carboxylate ligand [3], The three aromatic rings, C2-C3-C4-C5-C6-C7 (plane I I ) , C 1 3 C 1 4 C 1 5 C 1 6 C 1 7 C 1 8 (plane I I I ) , C20-C21-C22-C23-C24—C25 (plane IV) in the coordination cation are all well-defined planes. The dihedral angles between the metal basal plane I and the other three aromatic planes (Π, ΙΠ and IV) are respectively, 52.2°, 39.9°, and 37.6°. The dihedral angle between the two aromatic rings (Π and ΙΠ) in the same ligand is 13.9°, indicating that these two rings are almost parallel each other. All the oxygen and the nitrogen atoms in the complex contribute to the formation of hydrogen bonds. A great number of hydrogen bonds link the molecules into a two-dimensional network. First, the molecules are interconnected, in columns parallel to α-axis and then in layers parallel to ac-plane, by intermolecular hydrogen bonds. Table 1. Data collection and handling. blue block, size 0.32 χ 0.44 χ 0.48 mm Mo Ka radiation (0.71073 Â) 7.47 cnT Bruker SMART CCD, φ/ω 50.04° 8478, 5580 /obs > 2 a(Iobs), 3852 562 SHELXTL [5], SAD ABS [6] Crystal: Wavelength: /< Diffractometer, scan mode: 2ömn\: N(hkl)measured, N(hkl)„„¡que: Criterion for I0bs, N(hkl)it: N(param) refmed: Programs: Discussion Amine complexes with transition metals carboxylate represent an important branch in the field of coordination chemistry. Previously we reported some examples of this kind of complexes [ 1 -4]. The title compound consists of one coordination cation, one benzoate anion, and two lattice water molecules. In the cation, the Cu(l) atom is in a square-pyramidal environment and is Table 2. Atomic coordinates and displacement parameters (in  ). Correspondence author (e-mail: hlzhu@wist.edu.cn) Atom Site χ y ζ í/iso H(l) 2 Í -0.123(5) 0.938(4) 0.338(1) 0.06(1) H(2) 2 i 0.056(4) 0.891(4) 0.364(1) 0.05(1) H(3) 2 i 0.255(5) 1.201(4) 0.518(1) 0.05(1) H(4) li 0.007(6) 1.294(5) 0.532(2) 0.09(1) H(5) 2i -0.249(6) 1.243(5) 0.468(2) 0.09(1) 504 C U ( C 2 5 H 3 0 F 2 N 3 O 3 ) ( C 7 H 5 O 2 ) · 2 H 2 0 Table 2. Continued. Table 2. Continued. Atom Site X y ζ U ISO Atom Site X y 2 í/iso H(6) 2 i -0.240(5) 1.103(4) 0.389(1) 0.05(1) H(23) l i 0.456(4) 0.567(3) 0.190(1) 0.027(7) H(7) 2 i 0.263(4) 1.102(3) 0.337(1) 0.024(8) H(24) l i 0.203(4) 0.671(3) 0.386(1) 0.042(9) H(8) l i 0.142(4) 1.293(4) 0.329(1) 0.05(1) H(25) l i 0.244(5) 0.517(4) 0.447(1) 0.06(1) H(9) l i -0.036(5) 1.160(3) 0.296(1) 0.042(9) H(26) l i 0.488(5) 0.411(4) 0.449(1) 0.06(1) H(10) l i 0.144(4) 1.322(3) 0.239(1) 0.049(9) H(27) l i 0.679(5) 0.461(4) 0.383(1) 0.05(1) H ( l l ) l i 0.335(5) 1.294(4) 0.264(1) 0.05(1) H(28) l i 0.630(4) 0.609(3) 0.327(1) 0.029(9) H(12) l i 0.020(5) 1.064(3) 0.209(1) 0.040(9) H(29) l i 0.816(5) 0.303(4) 0.087(1) 0.07(1) H(13) l i 0.208(4) 1.161(3) 0.150(1) 0.040(8) H(30) l i 0.815(6) 0.196(5) 0.004(2) 0.09(1) H(14) l i 0.386(5) 1.165(3) 0.188(1) 0.044(9) H(31) l i 0.749(6) -0.065(5) -0.019(2) 0.10(2) H(15) l i 0.079(4) 0.879(3) 0.135(1) 0.032(8) H(32) l i 0.702(6) -0.236(5) 0.042(2) 0.09(1) H(16) l i 0.293(5) 0.937(4) 0.124(1) 0.06(1) H(33) l i 0.689(4) -0.126(4) 0.126(1) 0.05(1) H(17) l i 0.370(4) 0.874(3) 0.200(1) 0.020(8) H(34) l i -0.185(7) 0.671(3) 0.242(2) 0.10(1) H(18) l i 0.171(4) 0.619(3) 0.208(1) 0.046(9) H(35) l i -0.247(4) 0.801(4) 0.244(2) 0.09(2) H(19) l i 0.029(5) 0.641(3) 0.164(1) 0.047(9) H(36) l i 0.47(2) 0.858(7) 0.673(2) 0.10(2) H(20) l i 0.210(5) 0.478(4) 0.017(1) 0.06(1) H(37) l i 0.348(5) 0.744(2) 0.704(2) 0.09(2) H(21) l i 0.495(5) 0.408(4) 0.043(1) 0.07(1) H(38) l i 0.040(2) 0.474(6) 0.718(2) 0.09(1) H(22) l i 0.600(5) 0.458(4) 0.131(1) 0.06(1) H(39) l i 0.183(5) 0.590(4) 0.7568(9) 0.08(1) Table 3. Atomic coordinates and displacement parameters (in Â). Atom Site χ y ζ U\\ U22 í/33 U12 U13 U23 Cu(l) l i 0.17881(6) 0.92881(4) 0.25892(2) 0.0459(3) 0.0444(2) 0.0393(2) 0.0255(2) 0.0107(2) 0.0087(2) F( l ) l i 0.3133(3) 1.0625(3) 0.43937(9) 0.065(2) 0.101(2) 0.088(2) 0.040(1) 0.008(1) 0.017(1) F(2) l i 0.0346(3) 0.6045(3) 0.06964(8) 0.079(2) 0.105(2) 0.058(1) 0.050(1) -0.007(1) 0.003(1) N( l ) l i 0.1511(4) 1.0677(3) 0.3218(1) 0.036(2) 0.044(2) 0.043(2) 0.017(1) 0.005(1) 0.006(1) N(2) l i 0.1409(4) 1.0963(3) 0.2197(1) 0.036(2) 0.044(2) 0.046(2) 0.020(1) 0.005(1) 0.007(1) N(3) l i 0.2517(4) 0.8446(3) 0.1925(1) 0.034(2) 0.043(2) 0.040(2) 0.017(1) 0.006(1) 0.008(1) O ( l ) l i 0.2270(3) 0.7773(2) 0.30212(8) 0.049(1) 0.057(1) 0.047(1) 0.034(1) 0.018(1) 0.020(1) 0(2) l i 0.5206(3) 0.8062(3) 0.27984(9) 0.049(2) 0.078(2) 0.061(2) 0.034(1) 0.025(1) 0.036(1) 0(3) l i 0.7977(4) 0.3079(3) 0.1808(1) 0.087(2) 0.054(2) 0.078(2) 0.031(2) 0.012(2) 0.007(1) 0(4) l i 0.7047(3) 0.0614(3) 0.20213(9) 0.060(2) 0.065(2) 0.062(2) 0.026(1) 0.011(1) 0.015(1) 0(5) l i -0.1528(3) 0.7705(3) 0.2364(1) 0.040(2) 0.061(2) 0.077(2) 0.020(1) 0.012(1) -0.005(1) 0(6) l i 0.4199(4) 0.8424(3) 0.7024(1) 0.052(2) 0.075(2) 0.097(2) 0.024(2) 0.017(2) 0.025(2) 0(7) l i 0.1663(5) 0.5244(4) 0.7282(1) 0.080(2) 0.071(2) 0.091(2) 0.031(2) 0.039(2) 0.007(2) C( l ) l i 0.0150(6) 0.9793(4) 0.3560(1) 0.053(2) 0.049(2) 0.051(2) 0.020(2) 0.015(2) 0.003(2) C(2) l i 0.0129(5) 1.0744(4) 0.4061(1) 0.050(2) 0.049(2) 0.045(2) 0.019(2) 0.014(2) 0.007(2) C(3) l i 0.1601(5) 1.1104(4) 0.4467(1) 0.057(2) 0.053(2) 0.057(2) 0.018(2) 0.017(2) 0.013(2) C(4) l i 0.1615(8) 1.1904(5) 0.4940(2) 0.077(3) 0.069(3) 0.047(3) 0.010(2) 0.001(2) 0.012(2) C(5) l i 0.0075(9) 1.2387(6) 0.5009(2) 0.108(4) 0.075(3) 0.057(3) 0.030(3) 0.034(3) 0.001(2) C(6) l i -0.1421(8) 1.2057(6) 0.4617(2) 0.092(4) 0.086(3) 0.072(3) 0.049(3) 0.035(3) 0.003(3) C(7) l i -0.1403(7) 1.1251(5) 0.4146(2) 0.068(3) 0.087(3) 0.051(3) 0.042(2) 0.014(2) 0.007(2) C(8) l i 0.1013(6) 1.2026(4) 0.3035(1) 0.051(2) 0.043(2) 0.054(2) 0.025(2) 0.007(2) -0.002(2) C(9) l i 0.1938(6) 1.2466(4) 0.2559(1) 0.054(2) 0.037(2) 0.061(2) 0.024(2) 0.005(2) 0.006(2) C(10) l i 0.2472(6) 1.1045(4) 0.1749(1) 0.052(2) 0.051(2) 0.050(2) 0.026(2) 0.010(2) 0.018(2) C ( l l ) l i 0.2112(6) 0.9353(4) 0.1514(1) 0.051(2) 0.056(2) 0.040(2) 0.025(2) 0.008(2) 0.013(2) C(12) l i 0.1604(6) 0.6672(4) 0.1780(1) 0.046(2) 0.043(2) 0.044(2) 0.014(2) 0.009(2) 0.006(2) C(13) l i 0.2553(5) 0.5966(3) 0.1394(1) 0.043(2) 0.036(2) 0.039(2) 0.013(2) 0.010(2) 0.002(1) C(14) l i 0.1901(5) 0.5650(4) 0.0873(1) 0.049(2) 0.055(2) 0.048(2) 0.022(2) 0.003(2) 0.005(2) C(15) l i 0.2713(7) 0.4958(5) 0.0516(2) 0.080(3) 0.074(3) 0.040(2) 0.029(2) 0.007(2) -0.007(2) C(16) l i 0.4263(6) 0.4525(5) 0.0688(2) 0.075(3) 0.059(2) 0.062(3) 0.029(2) 0.027(2) -0.002(2) C(17) l i 0.4973(6) 0.4814(4) 0.1203(2) 0.058(3) 0.054(2) 0.072(3) 0.029(2) 0.016(2) 0.006(2) C(18) l i 0.4119(5) 0.5516(4) 0.1552(1) 0.055(2) 0.046(2) 0.043(2) 0.018(2) 0.005(2) 0.004(2) C(19) l i 0.3909(5) 0.7559(4) 0.3069(1) 0.045(2) 0.039(2) 0.038(2) 0.020(2) 0.008(2) 0.003(1) C(20) l i 0.4176(4) 0.6573(3) 0.3482(1) 0.043(2) 0.036(2) 0.035(2) 0.018(2) 0.004(1) 0.003(1) C(21) l i 0.3001(6) 0.6293(4) 0.3864(1) 0.059(2) 0.057(2) 0.047(2) 0.031(2) 0.015(2) 0.015(2) C(22) l ì 0.3279(7) 0.5390(5) 0.4244(2) 0.073(3) 0.072(3) 0.047(2) 0.028(2) 0.019(2) 0.022(2) C(23) l i 0.4706(6) 0.4751(4) 0.4236(2) 0.077(3) 0.054(2) 0.050(2) 0.022(2) -0.004(2) 0.019(2) C(24) l i 0.5885(6) 0.5017(4) 0.3858(2) 0.061(3) 0.053(2) 0.060(3) 0.033(2) 0.003(2) 0.013(2) 0(25) l i 0.5622(6) 0.5927(4) 0.3484(2) 0.052(2) 0.053(2) 0.045(2) 0.023(2) 0.012(2) 0.011(2) C(26) l i 0.7482(5) 0.1590(5) 0.1704(1) 0.035(2) 0.055(2) 0.064(2) 0.021(2) 0.004(2) 0.013(2) C(27) l i 0.7478(5) 0.0933(4) 0.1154(1) 0.037(2) 0.046(2) 0.060(2) 0.016(2) 0.009(2) 0.010(2) C(28) l i 0.7841(6) 0.1916(5) 0.0777(2) 0.086(3) 0.060(3) 0.075(3) 0.031(2) 0.023(2) 0.019(2) C(29) l i 0.7885(8) 0.1322(7) 0.0283(2) 0.127(5) 0.090(4) 0.076(4) 0.032(3) 0.036(3) 0.039(3) C(30) l i 0.7576(8) -0.0277(7) 0.0151(2) 0.104(4) 0.094(4) 0.065(3) 0.021(3) 0.024(3) 0.002(3) C(31) l i 0.7199(7) -0.1261(6) 0.0516(2) 0.090(3) 0.062(3) 0.079(3) 0.020(2) 0.019(3) -0.005(3) C(32) l i 0.7137(6) -0.0677(5) 0.1010(2) 0.064(3) 0.053(3) 0.066(3) 0.016(2) 0.012(2) 0.014(2) CU(C25H30F2N3O3)(C7H5O2) • 2 H 2 0 505 Acknowledgments. The authors thank the Education Office of Hubei Province, P. R. China, for the research grant No. 2002B29002 and the Natural Science Foundation of Hubei Province, P. R. China, for the research grant No. 2003ABB010.

Crystal structure of diaqua-trans-dicinnamato-dihexamethylene-tetraminecobalt(II)dihydrate,Co(C6H12N4)2(C9H7O2)2(H2O)2·2H2O

C30H46C0N8O8, monoclinic, P12i /c l (No. 14), a = 12.779(3) À, b = 10.938(2)À, c = 1 2 . 2 1 8 ( 2 ) Â , = 97.56(3)°, V= 1693.0À , Z = 2, Rgt(F) = 0.085, wRKf(F) = 0.201, T= 293 K. Source of material All reagents and solvents were used as obtained without further purification. C, Η and Ν elemental analyses were performed on a Perkin-Elmer elemental analyzer. Cobalt cinnamate dihydrate (1 mmol, 389 mg) and hexamethylenetetramine (1 mmol, 140 mg) were dissolved in ammonium solution (20 ml), and stirred for ca. 10 min to obtain a clear purple solution. After keeping the solution in air for two weeks with the ammonium gas escaping, large violet crystals were formed. This product was collected, washed three times with water, and dried in a vacuum desiccator using CaCb (yield 66%). Elemental analysis: found C, 50.88%; H, 6.66%; N, 15.70%; calc. for CaoHUeCoNgOg C, 51.06%; H. 6.57%; N, 15.8 Table 1. Data collection and handling. Experimental details The relative large R values are perhaps a result of a deficient absorption correction because the form of the crystal was irregular. Residual electron density: +0.843 e-Á, 0.792 e-À. All Η atoms were placed in geometrically idealised positions and constrained to ride on their parent atoms with Ν—Η and C—Η distances of 0.90 À and 0.96 A, respectively, and the UiS0 values for H atoms were fixed at 0.080. Although the C(2) atom was a little disordered (Ueq = 0.184(8)) we do not try to split it. Discussion Each of the title discrete complex consists of a diaqua-dicinnamato-dihexamethylenetetraminecobalt(II) coordination dication and two lattice water molecules. The central cobalt(II) Crystal:

Crystal structure of diaqua-dibenzoato-dihexamethylenetetraminenickel(II) dihydrate, Ni(C6H12N4)2(C7H5O2)2(H2O)2 · 2H2O

C26H42N8Ni08, monoclinic, C12/cl (No. 15), a = 22.784(5) A, b = 10.886(2)Â, c = 12.208(2)Â, = 95.50(3)°, V= 3014.0A3, Z = 4, Rgt(F) = 0.074, wRref(F2) = 0.156, T= 293 K. Source of material

Crystal structure of di(2-aminopyridine)-tetrakis[N-(2-aminopropyl)-salicylaldiminato)]tricobalt(III) diperchlorate, Co3(C58H48N12O4)(ClO4)2

Abstract C58H48Cl2Co3N12O12, triclinic, P1̅̅̅̅ (No. 2), a = 11.640(3) Å, b = 11.693(3) Å, c = 12.218(3) Å, α = 78.968(5)°, β = 89.827(5)°, γ = 60.605(4)°, V = 1414.0 Å3, Z = 1, Rgt(F) = 0.062, wRref(F2) = 0.136, T = 293 K.

Crystal structure of bis[dinitrato-2,5,8-triaza-1,9-di(2-fluorobenzylnonanecopper( II)] monohydrate, CU(C18H22F2N5O6)2 · H2O

Abstract C36H48Cu2F4N10O13, monoclinic, C1c1 (No. 9), a = 14.870(8) Å, b = 20.78(1) Å, c = 14.660(7) Å, β = 101.308(9)°, V = 4441.6 Å3, Z = 4, Rgt(F) = 0.053, wRref(F2) = 0.147, T = 298 K.