Literature DB >> 21754336

Aqua-chloridobis(diphenyl-glyoximato-κN,N')cobalt(III) dihydrate.

Parthasarathy Meera1, Madhavan Amutha Selvi, Arunachalam Dayalan.   

Abstract

The asymmetric unit of the title complex, [Co(C(14)H(11)N(2)O(2))(2)Cl(H(2)O)]·2H(2)O or [Co(dpgH)(2)Cl(H(2)O)]·2H(2)O, where dpgH(-) is diphenyl glyoximate, consists of one-half of a [Co(dpgH)(2)Cl(H(2)O)] complex and one solvent water mol-ecule. The complex is completed through inversion symmetry, with the Co(III) atom situated at the centre of symmetry. The coordination geometry around the Co(III) atom is distorted octa-hedral with the four N atoms of the two dpgH(-) ligands forming an approximate square plane with N-Co-N bite angles of 81.13 (14) and 98.87 (14)°. The Cl(-) ligand and the water mol-ecule are disordered in a 1:1 ratio and are in the axial positions, almost perpendicular to the plane of the glyoximate ligands [O-Co-Cl = 175.3 (10)°]. The two glyoximate ligands are linked by strong intra-molecular O-H⋯O hydrogen bonds. In addition, O-H⋯O inter-actions involving the solvent water mol-ecules and O-H⋯N hydrogen-bonding inter-actions are also observed. The solvent water mol-ecule is disordered over five positions with different occupancies.

Entities:  

Year:  2011        PMID： 21754336      PMCID： PMC3089102          DOI： 10.1107/S1600536811014280

Source DB:  PubMed          Journal:  Acta Crystallogr Sect E Struct Rep Online        ISSN： 1600-5368


Related literature

For related complexes, see: Gupta et al. (2003 ▶); Randaccio (1999 ▶); Brown & Satyanarayana (1992 ▶); Gilaberte et al. (1988 ▶). For the nature of equatorial ligands, see: Varhelyi et al. (1999 ▶). For similar structures, see: Meera et al. (2009 ▶). For details of the synthesis, see: Toscano et al. (1983 ▶); Gupta et al. (2001 ▶). For spectroscopic studies related to the complex, see: Gupta et al. (2004 ▶); Lopez et al. (1992 ▶); Silverstein & Bassler (1984 ▶); Mandal & Gupta (2005 ▶).

Experimental

Crystal data

[Co(C14H11N2O2)2Cl(H2O)]·2H2O M = 626.92 Monoclinic, a = 12.0709 (4) Å b = 5.9689 (2) Å c = 21.9224 (5) Å β = 104.770 (1)° V = 1527.32 (8) Å3 Z = 2 Mo Kα radiation μ = 0.70 mm−1 T = 293 K 0.30 × 0.20 × 0.20 mm

Data collection

Bruker APEXII CCD diffractometer Absorption correction: multi-scan (SADABS; Bruker, 1999 ▶) T min = 0.761, T max = 0.861 13610 measured reflections 2682 independent reflections 2431 reflections with I > 2σ(I) R int = 0.030

Refinement

R[F 2 > 2σ(F 2)] = 0.062 wR(F 2) = 0.199 S = 1.25 2682 reflections 215 parameters 1 restraint H-atom parameters constrained Δρmax = 0.92 e Å−3 Δρmin = −0.53 e Å−3 Data collection: APEX2 (Bruker, 2004 ▶); cell refinement: SAINT (Bruker, 2004 ▶); data reduction: SAINT; program(s) used to solve structure: SIR92 (Altomare et al., 1993 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: ORTEP-3 (Farrugia, 1997 ▶) and Mercury (Macrae et al., 2008 ▶); software used to prepare material for publication: PLATON (Spek, 2009 ▶). Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536811014280/wm2477sup1.cif Structure factors: contains datablocks I. DOI: 10.1107/S1600536811014280/wm2477Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report
[Co(C14H11N2O2)2Cl(H2O)]·2H2OF(000) = 648
Mr = 626.92Dx = 1.363 Mg m−3
Monoclinic, P21/nMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ynCell parameters from 2441 reflections
a = 12.0709 (4) Åθ = 2.8–25.0°
b = 5.9689 (2) ŵ = 0.70 mm−1
c = 21.9224 (5) ÅT = 293 K
β = 104.770 (1)°Block, brown
V = 1527.32 (8) Å30.30 × 0.20 × 0.20 mm
Z = 2
Bruker APEXII CCD diffractometer2682 independent reflections
Radiation source: fine-focus sealed tube2431 reflections with I > 2σ(I)
graphiteRint = 0.030
ω and φ scanθmax = 25.0°, θmin = 1.8°
Absorption correction: multi-scan (SADABS; Bruker, 1999)h = −14→14
Tmin = 0.761, Tmax = 0.861k = −7→7
13610 measured reflectionsl = −25→26
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.062H-atom parameters constrained
wR(F2) = 0.199w = 1/[σ2(Fo2) + (0.1021P)2 + 2.2574P] where P = (Fo2 + 2Fc2)/3
S = 1.25(Δ/σ)max < 0.001
2682 reflectionsΔρmax = 0.92 e Å−3
215 parametersΔρmin = −0.53 e Å−3
1 restraintExtinction correction: SHELXL97 (Sheldrick, 2008), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.025 (3)
Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.
Refinement. Refinement of F2 against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.
xyzUiso*/UeqOcc. (<1)
C10.3917 (4)0.0079 (7)0.0955 (2)0.0349 (9)
C20.5064 (3)0.0989 (7)0.12232 (19)0.0342 (9)
C30.3003 (4)0.0027 (8)0.1290 (2)0.0404 (11)
C40.2296 (4)−0.1819 (9)0.1254 (2)0.0519 (12)
H40.2423−0.30920.10370.062*
C50.1405 (5)−0.1770 (12)0.1539 (3)0.0668 (16)
H50.0927−0.30090.15080.080*
C60.1215 (5)0.0054 (12)0.1864 (3)0.0677 (18)
H60.06100.00620.20550.081*
C70.1911 (5)0.1880 (11)0.1913 (3)0.0619 (15)
H70.17840.31310.21390.074*
C80.2809 (4)0.1867 (9)0.1625 (2)0.0482 (11)
H80.32840.31120.16600.058*
C90.5534 (3)0.1512 (8)0.19009 (18)0.0353 (9)
C100.5471 (4)−0.0079 (8)0.2349 (2)0.0457 (11)
H100.5078−0.14120.22270.055*
C110.5994 (5)0.0313 (11)0.2977 (2)0.0576 (14)
H110.5969−0.07670.32790.069*
C120.6550 (4)0.2299 (11)0.3153 (2)0.0604 (16)
H120.69000.25590.35760.073*
C130.6600 (4)0.3909 (10)0.2718 (2)0.0519 (13)
H130.69720.52590.28440.062*
C140.6092 (4)0.3513 (8)0.2090 (2)0.0432 (11)
H140.61250.45990.17910.052*
N10.3780 (3)−0.0578 (6)0.03761 (16)0.0335 (8)
N20.5663 (3)0.1165 (6)0.08134 (15)0.0325 (8)
O10.2790 (2)−0.1374 (6)0.00398 (14)0.0455 (8)
O20.6748 (2)0.1866 (6)0.09899 (14)0.0416 (8)
H2A0.70250.18490.06850.10 (3)*
Co10.50000.00000.00000.0294 (3)
Cl10.5813 (10)−0.3227 (16)0.0360 (5)0.0429 (13)0.50
O30.564 (2)−0.296 (4)0.0254 (12)0.044 (7)0.50
O4A0.7645 (12)0.624 (3)0.0072 (7)0.084 (3)0.302 (9)
O4B0.9669 (16)0.417 (4)0.0424 (9)0.084 (3)0.250 (10)
O4C0.875 (3)0.618 (7)0.0176 (17)0.084 (3)0.131 (9)
O4D1.023 (2)0.437 (5)−0.0007 (13)0.084 (3)0.198 (9)
O4E1.002 (3)0.295 (9)0.028 (2)0.084 (3)0.119 (10)
U11U22U33U12U13U23
C10.033 (2)0.038 (2)0.034 (2)−0.0038 (17)0.0086 (17)−0.0021 (16)
C20.031 (2)0.037 (2)0.034 (2)−0.0015 (17)0.0082 (17)0.0000 (17)
C30.033 (2)0.054 (3)0.033 (2)−0.0056 (19)0.0075 (18)−0.0005 (18)
C40.054 (3)0.059 (3)0.046 (3)−0.016 (2)0.019 (2)−0.004 (2)
C50.054 (3)0.087 (4)0.064 (3)−0.030 (3)0.023 (3)0.003 (3)
C60.045 (3)0.109 (5)0.057 (3)−0.008 (3)0.027 (3)−0.003 (3)
C70.049 (3)0.083 (4)0.058 (3)0.010 (3)0.022 (2)−0.009 (3)
C80.039 (2)0.058 (3)0.050 (3)−0.002 (2)0.015 (2)−0.005 (2)
C90.0275 (19)0.046 (2)0.033 (2)0.0019 (18)0.0090 (16)−0.0058 (18)
C100.041 (3)0.057 (3)0.041 (2)0.002 (2)0.013 (2)−0.001 (2)
C110.053 (3)0.083 (4)0.036 (3)0.013 (3)0.011 (2)0.009 (2)
C120.038 (3)0.104 (5)0.035 (2)0.008 (3)0.002 (2)−0.020 (3)
C130.038 (2)0.067 (3)0.050 (3)−0.003 (2)0.011 (2)−0.023 (3)
C140.035 (2)0.053 (3)0.043 (2)−0.005 (2)0.0112 (18)−0.008 (2)
N10.0282 (17)0.0370 (18)0.0344 (18)−0.0050 (14)0.0061 (14)−0.0023 (15)
N20.0278 (17)0.0378 (19)0.0312 (16)−0.0044 (14)0.0061 (13)−0.0015 (14)
O10.0311 (15)0.065 (2)0.0411 (16)−0.0167 (15)0.0101 (13)−0.0096 (15)
O20.0272 (15)0.060 (2)0.0369 (15)−0.0128 (14)0.0064 (12)−0.0088 (14)
Co10.0256 (5)0.0331 (5)0.0286 (5)−0.0046 (3)0.0054 (3)−0.0011 (3)
Cl10.044 (3)0.0374 (18)0.041 (3)0.0015 (18)−0.001 (3)0.004 (2)
O30.027 (8)0.064 (12)0.031 (8)−0.003 (7)−0.012 (5)0.016 (5)
O4A0.062 (6)0.103 (9)0.087 (7)0.019 (6)0.021 (5)0.004 (6)
O4B0.062 (6)0.103 (9)0.087 (7)0.019 (6)0.021 (5)0.004 (6)
O4C0.062 (6)0.103 (9)0.087 (7)0.019 (6)0.021 (5)0.004 (6)
O4D0.062 (6)0.103 (9)0.087 (7)0.019 (6)0.021 (5)0.004 (6)
O4E0.062 (6)0.103 (9)0.087 (7)0.019 (6)0.021 (5)0.004 (6)
C1—N11.298 (6)C11—C121.368 (9)
C1—C21.463 (6)C11—H110.9300
C1—C31.473 (6)C12—C131.366 (8)
C2—N21.294 (5)C12—H120.9300
C2—C91.482 (6)C13—C141.377 (6)
C3—C81.375 (7)C13—H130.9300
C3—C41.383 (7)C14—H140.9300
C4—C51.375 (7)N1—O11.323 (4)
C4—H40.9300N1—Co11.894 (3)
C5—C61.353 (9)N2—O21.334 (4)
C5—H50.9300N2—Co11.891 (3)
C6—C71.363 (9)O2—H2A0.8200
C6—H60.9300Co1—N2i1.891 (3)
C7—C81.386 (7)Co1—N1i1.894 (3)
C7—H70.9300Co1—O31.95 (3)
C8—H80.9300Co1—O3i1.95 (3)
C9—C141.382 (6)Co1—Cl12.214 (11)
C9—C101.382 (6)Co1—Cl1i2.214 (11)
C10—C111.381 (7)O4D—O4Dii0.94 (4)
C10—H100.9300
O4A···O3iii2.592 (4)O4A···CL1iii2.470 (2)
O4A···O1i2.951 (2)
N1—C1—C2112.1 (4)C13—C14—C9120.5 (5)
N1—C1—C3123.8 (4)C13—C14—H14119.8
C2—C1—C3124.0 (4)C9—C14—H14119.8
N2—C2—C1113.0 (4)C1—N1—O1121.7 (3)
N2—C2—C9122.6 (4)C1—N1—Co1116.8 (3)
C1—C2—C9124.2 (4)O1—N1—Co1121.0 (3)
C8—C3—C4118.7 (4)C2—N2—O2120.4 (3)
C8—C3—C1120.1 (4)C2—N2—Co1116.6 (3)
C4—C3—C1121.2 (4)O2—N2—Co1122.5 (2)
C5—C4—C3120.0 (5)N2—O2—H2A109.5
C5—C4—H4120.0N2—Co1—N2i179.998 (1)
C3—C4—H4120.0N2—Co1—N181.13 (14)
C6—C5—C4120.9 (5)N2i—Co1—N198.87 (14)
C6—C5—H5119.5N2—Co1—N1i98.87 (14)
C4—C5—H5119.5N2i—Co1—N1i81.13 (14)
C5—C6—C7120.1 (5)N1—Co1—N1i180.00 (17)
C5—C6—H6120.0N2—Co1—O391.3 (7)
C7—C6—H6120.0N2i—Co1—O388.7 (7)
C6—C7—C8119.8 (5)N1—Co1—O390.4 (9)
C6—C7—H7120.1N1i—Co1—O389.6 (9)
C8—C7—H7120.1N2—Co1—O3i88.7 (7)
C3—C8—C7120.5 (5)N2i—Co1—O3i91.3 (7)
C3—C8—H8119.7N1—Co1—O3i89.6 (9)
C7—C8—H8119.7N1i—Co1—O3i90.4 (9)
C14—C9—C10119.5 (4)O3—Co1—O3i179.999 (2)
C14—C9—C2121.0 (4)N2—Co1—Cl186.6 (3)
C10—C9—C2119.4 (4)N2i—Co1—Cl193.4 (3)
C11—C10—C9119.9 (5)N1—Co1—Cl190.6 (3)
C11—C10—H10120.1N1i—Co1—Cl189.4 (3)
C9—C10—H10120.1O3—Co1—Cl14.7 (10)
C12—C11—C10119.6 (5)O3i—Co1—Cl1175.3 (10)
C12—C11—H11120.2N2—Co1—Cl1i93.4 (3)
C10—C11—H11120.2N2i—Co1—Cl1i86.6 (3)
C13—C12—C11121.3 (4)N1—Co1—Cl1i89.4 (3)
C13—C12—H12119.4N1i—Co1—Cl1i90.6 (3)
C11—C12—H12119.4O3—Co1—Cl1i175.3 (10)
C12—C13—C14119.3 (5)O3i—Co1—Cl1i4.7 (10)
C12—C13—H13120.3Cl1—Co1—Cl1i179.999 (1)
C14—C13—H13120.3
N1—C1—C2—N26.6 (5)C1—C2—N2—O2−176.8 (3)
C3—C1—C2—N2−170.3 (4)C9—C2—N2—O2−0.8 (6)
N1—C1—C2—C9−169.3 (4)C1—C2—N2—Co1−5.3 (5)
C3—C1—C2—C913.8 (7)C9—C2—N2—Co1170.7 (3)
N1—C1—C3—C8−132.9 (5)C2—N2—Co1—N2i164 (6)
C2—C1—C3—C843.6 (6)O2—N2—Co1—N2i−25 (6)
N1—C1—C3—C444.5 (7)C2—N2—Co1—N12.1 (3)
C2—C1—C3—C4−139.0 (5)O2—N2—Co1—N1173.5 (3)
C8—C3—C4—C51.4 (7)C2—N2—Co1—N1i−177.9 (3)
C1—C3—C4—C5−176.0 (5)O2—N2—Co1—N1i−6.5 (3)
C3—C4—C5—C6−0.9 (8)C2—N2—Co1—O3−88.1 (10)
C4—C5—C6—C70.0 (9)O2—N2—Co1—O383.2 (10)
C5—C6—C7—C80.4 (9)C2—N2—Co1—O3i91.9 (10)
C4—C3—C8—C7−1.0 (7)O2—N2—Co1—O3i−96.8 (10)
C1—C3—C8—C7176.4 (4)C2—N2—Co1—Cl1−89.0 (4)
C6—C7—C8—C30.1 (8)O2—N2—Co1—Cl182.4 (4)
N2—C2—C9—C1450.7 (6)C2—N2—Co1—Cl1i91.0 (4)
C1—C2—C9—C14−133.8 (4)O2—N2—Co1—Cl1i−97.6 (4)
N2—C2—C9—C10−125.5 (5)C1—N1—Co1—N22.0 (3)
C1—C2—C9—C1050.0 (6)O1—N1—Co1—N2174.3 (3)
C14—C9—C10—C11−1.9 (7)C1—N1—Co1—N2i−178.0 (3)
C2—C9—C10—C11174.4 (4)O1—N1—Co1—N2i−5.7 (3)
C9—C10—C11—C121.4 (7)C1—N1—Co1—N1i−133 (100)
C10—C11—C12—C13−0.1 (8)O1—N1—Co1—N1i39 (100)
C11—C12—C13—C14−0.8 (7)C1—N1—Co1—O393.2 (8)
C12—C13—C14—C90.2 (7)O1—N1—Co1—O3−94.5 (8)
C10—C9—C14—C131.1 (6)C1—N1—Co1—O3i−86.8 (8)
C2—C9—C14—C13−175.1 (4)O1—N1—Co1—O3i85.5 (8)
C2—C1—N1—O1−177.4 (4)C1—N1—Co1—Cl188.4 (4)
C3—C1—N1—O1−0.5 (6)O1—N1—Co1—Cl1−99.2 (4)
C2—C1—N1—Co1−5.1 (5)C1—N1—Co1—Cl1i−91.6 (4)
C3—C1—N1—Co1171.8 (3)O1—N1—Co1—Cl1i80.8 (4)
D—H···AD—HH···AD···AD—H···A
O2—H2A···O1i0.821.682.477 (4)162.
O2—H2A···N1i0.822.402.999 (4)130.
O4A—···.O3iii..2.592 (4).
Table 1

Selected bond lengths (Å)

Co1—N2i1.891 (3)
Co1—N1i1.894 (3)
Co1—O31.95 (3)
Co1—Cl12.214 (11)

Symmetry code: (i) .

Table 2

Hydrogen-bond geometry (Å, °)

D—H⋯AD—HH⋯AD⋯AD—H⋯A
O2—H2A⋯O1i0.821.682.477 (4)162
O2—H2A⋯N1i0.822.402.999 (4)130
O4A⋯O3ii  2.592 (4) 

Symmetry codes: (i) ; (ii) .

  3 in total

1.  A short history of SHELX.

Authors:  George M Sheldrick
Journal:  Acta Crystallogr A       Date:  2007-12-21       Impact factor: 2.290

2.  Chloridobis[diphenyl-glyoximato(1-)-κN,N'](1H-imidazole-κN)cobalt(III) hemihydrate.

Authors:  P Meera; C Revathi; A Dayalan
Journal:  Acta Crystallogr Sect E Struct Rep Online       Date:  2009-01-08

3.  Structure validation in chemical crystallography.

Authors:  Anthony L Spek
Journal:  Acta Crystallogr D Biol Crystallogr       Date:  2009-01-20
  3 in total

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