Home Physical Sciences Crystal structure of (6,6′-(((((2-aminoethyl)azanediyl)bis(ethane-2,1-diyl))bis(azanylylidene))bis(methanylylidene))bis(2,4-dichlorophenolato)-κ6N,N′,N′′,N′′′,O,O′)cadmium(II) – ethanol – water (1/1/1), C22H28CdCl4N4O4
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Crystal structure of (6,6′-(((((2-aminoethyl)azanediyl)bis(ethane-2,1-diyl))bis(azanylylidene))bis(methanylylidene))bis(2,4-dichlorophenolato)-κ6N,N′,N′′,N′′′,O,O′)cadmium(II) – ethanol – water (1/1/1), C22H28CdCl4N4O4

  • Zong-Li Ren , Ling-Zhi Liu , Yang Zhang and Wen-Kui Dong EMAIL logo
Published/Copyright: June 27, 2018

Abstract

C22H28CdCl4N4O4, monoclinic, C2/c (no. 15), a = 18.5053(5) Å, b = 13.0864(4) Å, c = 23.0284(9) Å, β = 102.367(3)°, V = 5447.4(3) Å3, Z = 8, Rgt(F) = 0.0457, wRref(F2) = 0.1306, T = 290.7(2) K.

CCDC no.: 1588661

The crystal structure is shown in the figure. Tables 1 and 2 contain details on crystal structure and measurement conditions and a list of the atoms including atomic coordinates and displacement parameters.

Table 1:

Data collection and handling.

Crystal:Clear light yellow block
Size:0.31 × 0.30 × 0.28 mm
Wavelength:Cu Kα radiation (1.54184 Å)
μ:10.3 mm−1
Diffractometer, scan mode:SuperNova, Dual, ω
θmax, completeness:70.6°, >99%
N(hkl)measured, N(hkl)unique, Rint:11751, 5146, 0.043
Criterion for Iobs, N(hkl)gt:Iobs > 2 σ(Iobs), 4267
N(param)refined:318
Programs:CrysAlisPRO [19], SHELX [20], OLEX2 [21]
Table 2:

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2).

AtomxyzUiso*/Ueq
Cd10.06207(2)0.57998(2)0.18699(2)0.03468(12)
Cl1−0.19328(7)0.52653(11)0.07922(7)0.0644(4)
Cl2−0.15304(9)0.12334(12)0.04771(8)0.0730(4)
Cl3−0.12140(8)0.87322(11)0.13768(6)0.0636(4)
Cl4−0.17783(10)0.76241(14)−0.09167(8)0.0883(5)
O1−0.05088(15)0.5151(2)0.16083(16)0.0472(8)
O20.00451(16)0.7323(2)0.14995(13)0.0414(7)
N10.0848(2)0.4079(3)0.20901(19)0.0420(9)
N20.20079(19)0.5489(3)0.20587(17)0.0433(9)
N30.0970(2)0.6008(3)0.09861(18)0.0486(10)
N40.10988(18)0.6681(3)0.27025(16)0.0405(8)
H4A0.08250.72320.27260.049*
H4B0.11020.62940.30210.049*
C1−0.0705(2)0.4278(3)0.1367(2)0.0380(9)
C2−0.1395(2)0.4165(4)0.0960(2)0.0434(10)
C3−0.1652(3)0.3255(4)0.0697(2)0.0505(12)
H3−0.21090.32250.04350.061*
C4−0.1230(3)0.2396(4)0.0823(2)0.0508(12)
C5−0.0549(3)0.2434(4)0.1216(2)0.0500(12)
H5−0.02680.18420.13030.060*
C6−0.0282(2)0.3362(4)0.1482(2)0.0427(10)
C70.0452(3)0.3313(4)0.1876(2)0.0480(11)
H70.06470.26660.19800.058*
C80.1592(2)0.3882(4)0.2447(2)0.0479(11)
H8A0.16810.31520.24770.057*
H8B0.16330.41530.28440.057*
C90.2160(2)0.4390(4)0.2153(2)0.0480(11)
H9A0.26500.42990.24020.058*
H9B0.21530.40640.17730.058*
C100.2236(3)0.5879(5)0.1532(3)0.0577(15)
H10A0.27230.56150.15210.069*
H10B0.22680.66180.15520.069*
C110.1694(3)0.5566(5)0.0971(2)0.0630(16)
H11A0.18610.58140.06240.076*
H11B0.16580.48280.09470.076*
C120.0547(3)0.6334(4)0.0509(2)0.0536(13)
H120.07010.62170.01560.064*
C13−0.0142(2)0.6865(4)0.0465(2)0.0428(10)
C14−0.0337(2)0.7371(3)0.09597(19)0.0398(9)
C15−0.0987(2)0.7992(4)0.0812(2)0.0434(10)
C16−0.1426(3)0.8064(4)0.0254(2)0.0539(12)
H16−0.18510.84640.01850.065*
C17−0.1227(3)0.7531(4)−0.0206(2)0.0548(13)
C18−0.0586(3)0.6965(4)−0.0112(2)0.0531(12)
H18−0.04450.6645−0.04310.064*
C190.2316(2)0.6072(4)0.2604(2)0.0487(11)
H19A0.28120.62970.25910.058*
H19B0.23530.56260.29460.058*
C200.1858(2)0.6985(4)0.2683(2)0.0486(11)
H20A0.20820.73340.30490.058*
H20B0.18460.74560.23560.058*
O30.1020(4)0.8942(6)0.1763(3)0.136(3)
H3A0.06140.86640.17020.203*
C210.0683(6)0.9796(9)0.0831(5)0.141(4)
H21A0.09021.01550.05490.212*
H21B0.05011.02800.10780.212*
H21C0.02810.93830.06240.212*
C220.1224(6)0.9160(7)0.1191(6)0.126(4)
H22A0.17010.94970.12620.151*
H22B0.12630.85240.09840.151*
O40.4285(5)0.5694(6)0.2513(5)0.198(4)
H4C0.46220.58550.28020.297*
H4D0.40670.51190.24590.297*

Source of material

[2-Aminotriethylamine-2′,2′′-bis(nitrilomethylidyne)]-4,4′,6,6′-tetrachloro-3,3′-diphenol (H2L) was synthesized by the reaction of tris(2-aminoethyl) amine and 3,5-dichlorosalicylaldehyde. Then, a solution of Cd(II) acetate hydrate (2.67 mg, 0.01 mmol) in ethanol (2 mL) was added dropwise to a solution of H2L (4.92 mg, 0.01 mmol) in chloroform (3 mL) at room temperature, the color turned yellow immediately. The mixture was filtered and was allowed to stand at room temperature for about 2 weeks. The light-yellow block crystals were obtained. Yield: 57.7%. Anal. calcd. for C22H28CdCl4N4O4: C, 39.63%; H, 4.23%; N, 8.40%. Found: C, 39.74%; H, 4.11%; N, 8.29%.

Experimental details

Hydrogen atoms were placed in their geometrically idealized positions and constrained to ride on their parent atoms.

Comment

The coordination chemistry of metal complexes with salen-type tetradentate ligands has achieved a considerable attention in the past decades [1], [2], [3], [4]. Many salen-type metal complexes have already been used in areas, such as the biological system [5], [6], [7], optical and magnetic materials [8], [9], [10], [11] and supramolecular architectures [12], [13], [14], [15], [16], [17].

The X-ray crystal structure determination shows that the title compound consists of one Cd(II) atom (Cd1), one double deprotonated (L)2− unit and one uncoordinated ethanol molecule and one water molecule. The Cd1 atom is hexa-coordinated by two deprotonated phenoxo oxygen atoms (O1 and O2) and four nitrogen atoms (N1, N2, N3 and N4) from the (L)2− Ligand. The coordination environment around Cd1 is a slightly distorted octahedral geometry (cf. the figure). Bond lengths and angles are all in the expected ranges [18].

References

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Received: 2018-03-07
Accepted: 2018-06-06
Published Online: 2018-06-27
Published in Print: 2018-08-28

©2018 Zong-Li Ren et al., published by De Gruyter, Berlin/Boston

This work is licensed under the Creative Commons Attribution-NonCommercial-NoDerivatives 4.0 License.

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  54. Crystal structure of 4-(dimethylamino)-1-(prop-2-yn-1-yl)pyridin-1-ium perchlorate, C10H13ClN2O4
  55. Crystal structure of 2-amino-5-oxo-4-(4-chloro-phenyl)-4,5,6,7-tetrahydro-cyclopenta[b]pyran-3-carbonitrile, C15H11ClN2O2
  56. Crystal structure of triaqua-(pyridine-2,6-dicarboxylato-κ3O,N,O′)cobalt(II) – 6-phenyl-1,3,5-triazine-2,4-diamine (1/1), C16H18CoN6O7
  57. Crystal structure of ethyl 2-amino-4-(3-cyanophenyl)-7,7-dimethyl-5-oxo-5,6,7,8-tetrahydro-4H-chromene-3-carboxylate, C21H22N2O4
  58. Crystal structure of 2-(4-chloro-2,6-dinitrophenyl)-1-(4-chloro-3-nitrophenyl)diazene 1-oxide, C12H5Cl2N5O7
  59. Crystal structure of 3,4-dimethyl-2,6-dinitrophenol, C8H8N2O5
  60. Crystal structure of 1,2-dimethyl-3,5-dinitrobenzene, C8H8N2O4
  61. Crystal structure of ethyl 4-(3-chlorophenyl)-2,7,7-trimethyl-5-oxo-1,4,5,6,7,8-hexahydroquinoline-3-carboxylate, C21H24ClNO3
  62. Crystal structure of N-(4-chlorophenyl)-2-(2,6-dichlorophenyl)acetamide, C14H10Cl3NO
  63. Crystal structure of 2-amino-4-(4-fluorophenyl)-3-cyano-5-oxo-4H,5H-pyrano[3,2c] chromene, C19H11FN2O3
  64. The crystal structure of (4-nitrophenyl) (5-ferrocenyl-3-(trifluoromethyl)-1H-pyrazol-1-yl) methanone, C21H12F3FeN3O3
  65. Crystal structure of 5,5′-((3-hydroxy-4-methoxyphenyl)methylene)bis(1,3-diethyl-6-hydroxy-2-thioxo-2,3-dihydropyrimidin-4(1H)-one), C24H30N4O6S2
  66. Crystal structure of (3aR,4R,5R,7R,8S,9R,9aS,12R)-7-ethyl-5-(1-hydroxy-2-((R)-3-hydroxypyrrolidin-1-yl)ethoxy)-4,7,9,12-tetramethyldecahydro-4,9a-propanocyclopenta[8]annulene-3,8-diol – a pleuromutilin derivative, C26H41NO5
  67. Crystal structure of bis(μ2-3-formyl-5-methoxy-2-oxidobenzoato-κ3O,O′:O′)-hexapyridine-dicadmium(II) – pyridine (1/1), C53H47Cd2N7O10
  68. Crystal structure of ethyl 2-amino-4-(3-methoxyphenyl)-5-oxo-4H,5H-pyrano[3,2-c]chromene-3-carboxylate, C22H19NO6
  69. Crystal structure of methyl 4-(3,5-ditrifluoromethylphenyl)-2,7,7-trimethyl-5-oxo-1,4,5,6,7,8-hexahydroquinoline-3-carboxylate — water (2/1), C22H21F6NO3
  70. Crystal structure of 2-(4-bromophenyl)-2,3-dihydro-1H-perimidine, C17H13BrN2
  71. Crystal structure of (5-ethyl-2-(4-methoxyphenyl)-1,3-dioxan-5-yl)methanol, C14H20O4
  72. Crystal structure of (E)-N-(4-bromo-2-(1-(hydroxyimino)ethyl)phenyl)benzamide, C15H13BrN2O2
  73. Crystal structure of caffeinium triiodide – caffeine (1/1), C16H21I3N8O4
  74. Crystal structure of methyl 2-methyl-4-(3-methoxyphenyl)-5-oxo-1,4,5,6,7,8-hexahydroquinoline-3-carboxylate, C19H21NO4
  75. Crystal structure of (E)-3-(3,5-di-tert-butyl-4-hydroxyphenyl)-1-phenylprop-2-en-1-one, C23H28O2
  76. Crystal structure of 1,4-bis(2-azidoethyl)piperazine-1,4-diium dichloride, C8H18N8Cl2
  77. The crystal structure of dichlorido-(1,3-bis(2,6-dimethylphenyl)-1H-imidazol-2(3H)-ylidene)-(morpholine-κ1N)palladium(II), C23H29Cl2N3OPd(II)
  78. The crystal structure of 1-((5-chloro-3-methyl-1-phenyl-1H-pyrazole-4-yl)methyl)-1,3-diphenylurea, C24H21ClN4O
  79. Crystal structure of 6-(2-bromoacetamido)tetrahydro-2H-pyran-2,3,4,5-Tetrayl tetraacetate, C16H22BrNO10
  80. Crystal structure of 5-methylpyrazine-2-carbohydrazide, C6H8N4O
  81. Crystal structure of catena-poly[(μ2-5-(tert-butyl)isophthalato-κ4O,O′:O′′,O′′′)(-4′-(pyridin-4-yl)-2,2′:6′,2′′-terpyridine-κ3N,N′,N′′)manganese(II)], C32H28N4O5Mn
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