Literature DB >> 23634002

cis-Chlorido(methyl-amine)-bis-(propane-1,3-diamine)-cobalt(III) dichloride monohydrate.

Velusamy Maheshwaran1, Munisamy Manjunathan, Krishnamoorthy Anbalagan, Viswanathan Thiruselvam, Mondikalipudur Nanjappagounder Ponnuswamy.   

Abstract

In the title compound, [n class="Chemical">CoCl(CH5N)(C3H10N2)2]Cl2·H2O, the Co(III) ion has an octa-hedral coordination environment and is surrounded by four N atoms of two propane-1,3-diamine ligands in the equatorial plane, with another N atom of the methylamine ligand and a Cl atom occupying the axial positions. The crystal packing is stabilized by inter-molecular N-H⋯O, N-H⋯Cl, and O-H⋯Cl inter-actions, generating a three-dimensional network.

Entities:  

Year:  2013        PMID： 23634002      PMCID： PMC3629484          DOI： 10.1107/S1600536813006442

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


Related literature

For the linear solvation energy relationship (LSER) method, see: Anbalagan (2011 ▶); Anbalagan et al. (2003 ▶, 2011 ▶). For the biological properties of cobalt(III) complexes, see: Chang et al. (2010 ▶). For related structures, see: Anbalagan et al. (2009 ▶); Lee et al. (2007 ▶); Ramesh et al. (2008 ▶); Ravichandran et al. (2009 ▶). For the preparation of (1,3-diamino­propane)­cobalt(III), see: Bailar & Work (1946 ▶).

Experimental

Crystal data

[CoCl(CH5N)(C3H10N2)2]Cl2·H2O M = 362.62 Triclinic, a = 7.4752 (6) Å b = 7.9065 (6) Å c = 14.4663 (13) Å α = 76.022 (6)° β = 76.907 (7)° γ = 73.779 (4)° V = 784.96 (11) Å3 Z = 2 Mo Kα radiation μ = 1.60 mm−1 T = 292 K 0.35 × 0.35 × 0.35 mm

Data collection

Oxford Diffraction Xcalibur Eos diffractometer Absorption correction: multi-scan (CrysAlis PRO; Oxford Diffraction, 2009 ▶) T min = 0.798, T max = 1.000 5020 measured reflections 2764 independent reflections 2071 reflections with I > 2σ(I) R int = 0.027

Refinement

R[F 2 > 2σ(F 2)] = 0.030 wR(F 2) = 0.055 S = 0.92 2764 reflections 162 parameters H atoms treated by a mixture of independent and constrained refinement Δρmax = 0.32 e Å−3 Δρmin = −0.28 e Å−3 Data collection: CrysAlis CCD (Oxford Diffraction, 2009 ▶); cell refinement: CrysAlis RED (Oxford Diffraction, 2009 ▶); data reduction: CrysAlis RED; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: ORTEP-3 for Windows (Farrugia, 2012 ▶) and PLATON (Spek, 2009 ▶); software used to prepare material for publication: PLATON. Click here for additional data file. Crystal structure: contains datablock(s) global, I. DOI: 10.1107/S1600536813006442/bt6894sup1.cif Click here for additional data file. Structure factors: contains datablock(s) I. DOI: 10.1107/S1600536813006442/bt6894Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report
[CoCl(CH5N)(C3H10N2)2]Cl2·H2OZ = 2
Mr = 362.62F(000) = 380
Triclinic, P1Dx = 1.534 Mg m−3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 7.4752 (6) ÅCell parameters from 2764 reflections
b = 7.9065 (6) Åθ = 2.8–25.0°
c = 14.4663 (13) ŵ = 1.60 mm−1
α = 76.022 (6)°T = 292 K
β = 76.907 (7)°Block, violet
γ = 73.779 (4)°0.35 × 0.35 × 0.35 mm
V = 784.96 (11) Å3
Oxford Diffraction Xcalibur Eos diffractometer2764 independent reflections
Radiation source: Enhance(Mo)X-ray Source2071 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.027
ω scansθmax = 25.0°, θmin = 2.7°
Absorption correction: multi-scan (CrysAlis PRO; Oxford Diffraction, 2009)h = −8→8
Tmin = 0.798, Tmax = 1.000k = −6→9
5020 measured reflectionsl = −17→16
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.030Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.055H atoms treated by a mixture of independent and constrained refinement
S = 0.92w = 1/[σ2(Fo2) + (0.0217P)2] where P = (Fo2 + 2Fc2)/3
2764 reflections(Δ/σ)max = 0.001
162 parametersΔρmax = 0.32 e Å−3
0 restraintsΔρmin = −0.28 e Å−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*/Ueq
C10.3821 (4)0.4046 (4)0.7738 (2)0.0358 (7)
H1A0.45130.49430.73850.043*
H1B0.30860.44440.83240.043*
C20.2490 (4)0.3907 (4)0.7126 (2)0.0367 (7)
H2A0.19120.29120.74410.044*
H2B0.14900.49970.70740.044*
C30.3492 (4)0.3631 (4)0.61316 (19)0.0346 (7)
H3A0.25610.37840.57290.042*
H3B0.42050.45400.58500.042*
C40.8945 (4)−0.1858 (4)0.8474 (2)0.0381 (7)
H4A0.9755−0.19100.89220.046*
H4B0.9572−0.27800.80920.046*
C50.7081 (4)−0.2246 (4)0.90423 (19)0.0368 (7)
H5A0.7331−0.32730.95610.044*
H5B0.6347−0.12230.93310.044*
C60.5945 (4)−0.2629 (4)0.84015 (19)0.0328 (7)
H6A0.6729−0.35730.80640.039*
H6B0.4873−0.30570.88040.039*
C70.8086 (4)−0.2353 (4)0.5976 (2)0.0394 (8)
H7A0.9010−0.27690.54490.059*
H7B0.6842−0.22590.58630.059*
H7C0.8299−0.31880.65670.059*
N10.5177 (3)0.2334 (3)0.80003 (14)0.0256 (5)
H1C0.45340.16360.84640.031*
H1D0.60200.25730.82770.031*
N20.4793 (3)0.1835 (3)0.61329 (15)0.0243 (5)
H2C0.54520.18370.55290.029*
H2D0.40700.10450.62400.029*
N30.5246 (3)−0.1013 (3)0.76779 (14)0.0226 (5)
H3C0.4124−0.04370.79710.027*
H3D0.4999−0.14260.72040.027*
N40.8692 (3)−0.0082 (3)0.78236 (15)0.0273 (5)
H4C0.9792−0.00750.74120.033*
H4D0.85490.07320.81910.033*
N50.8253 (3)−0.0572 (3)0.60532 (14)0.0251 (5)
H5C0.81200.01390.54730.030*
H5D0.9456−0.07150.61210.030*
O10.2225 (3)0.0443 (4)0.91094 (19)0.0487 (6)
Cl10.81500 (9)0.30498 (10)0.62727 (5)0.03471 (19)
Cl20.81288 (10)0.28479 (10)0.92550 (5)0.0405 (2)
Cl30.27376 (8)−0.14018 (9)0.61638 (5)0.02962 (18)
Co10.66519 (4)0.08437 (5)0.70286 (3)0.01944 (10)
H1E0.208 (5)−0.031 (5)0.960 (3)0.085 (16)*
H1F0.112 (5)0.118 (5)0.915 (2)0.074 (13)*
U11U22U33U12U13U23
C10.0395 (17)0.0269 (19)0.038 (2)0.0020 (14)−0.0084 (14)−0.0098 (15)
C20.0274 (15)0.035 (2)0.0400 (19)0.0078 (13)−0.0095 (13)−0.0063 (15)
C30.0406 (17)0.0266 (19)0.0338 (19)−0.0012 (14)−0.0166 (14)0.0013 (15)
C40.0400 (17)0.036 (2)0.039 (2)−0.0008 (14)−0.0218 (14)−0.0033 (16)
C50.0546 (19)0.030 (2)0.0233 (17)−0.0063 (15)−0.0166 (14)0.0051 (14)
C60.0447 (17)0.0234 (18)0.0310 (18)−0.0128 (14)−0.0097 (13)0.0023 (14)
C70.0360 (16)0.039 (2)0.047 (2)−0.0105 (15)0.0020 (14)−0.0226 (16)
N10.0262 (12)0.0290 (15)0.0244 (13)−0.0090 (11)−0.0051 (10)−0.0071 (11)
N20.0257 (11)0.0249 (15)0.0224 (13)−0.0057 (10)−0.0058 (9)−0.0036 (11)
N30.0265 (11)0.0235 (14)0.0193 (13)−0.0077 (10)−0.0049 (9)−0.0040 (11)
N40.0233 (11)0.0304 (16)0.0291 (14)−0.0042 (10)−0.0070 (10)−0.0077 (12)
N50.0210 (11)0.0279 (15)0.0254 (13)−0.0042 (10)−0.0043 (9)−0.0047 (11)
O10.0358 (14)0.0492 (18)0.0457 (16)−0.0074 (12)0.0087 (11)0.0023 (13)
Cl10.0364 (4)0.0318 (5)0.0377 (5)−0.0194 (3)−0.0022 (3)−0.0007 (4)
Cl20.0464 (4)0.0318 (5)0.0444 (5)−0.0038 (4)−0.0175 (4)−0.0069 (4)
Cl30.0260 (4)0.0332 (5)0.0315 (4)−0.0087 (3)−0.0089 (3)−0.0039 (3)
Co10.01893 (18)0.0188 (2)0.0209 (2)−0.00540 (15)−0.00410 (14)−0.00248 (16)
C1—N11.471 (3)C7—H7A0.9600
C1—C21.514 (3)C7—H7B0.9600
C1—H1A0.9700C7—H7C0.9600
C1—H1B0.9700N1—Co11.988 (2)
C2—C31.500 (4)N1—H1C0.9000
C2—H2A0.9700N1—H1D0.9000
C2—H2B0.9700N2—Co11.9854 (19)
C3—N21.480 (3)N2—H2C0.9000
C3—H3A0.9700N2—H2D0.9000
C3—H3B0.9700N3—Co11.9722 (18)
C4—N41.478 (3)N3—H3C0.9000
C4—C51.520 (4)N3—H3D0.9000
C4—H4A0.9700N4—Co11.987 (2)
C4—H4B0.9700N4—H4C0.9000
C5—C61.519 (3)N4—H4D0.9000
C5—H5A0.9700N5—Co11.9815 (19)
C5—H5B0.9700N5—H5C0.9000
C6—N31.493 (3)N5—H5D0.9000
C6—H6A0.9700O1—H1E0.82 (4)
C6—H6B0.9700O1—H1F0.87 (4)
C7—N51.480 (3)Cl1—Co12.2599 (7)
N1—C1—C2112.7 (2)Co1—N1—H1C106.8
N1—C1—H1A109.0C1—N1—H1D106.8
C2—C1—H1A109.0Co1—N1—H1D106.8
N1—C1—H1B109.0H1C—N1—H1D106.7
C2—C1—H1B109.0C3—N2—Co1121.69 (15)
H1A—C1—H1B107.8C3—N2—H2C106.9
C3—C2—C1111.9 (2)Co1—N2—H2C106.9
C3—C2—H2A109.2C3—N2—H2D106.9
C1—C2—H2A109.2Co1—N2—H2D106.9
C3—C2—H2B109.2H2C—N2—H2D106.7
C1—C2—H2B109.2C6—N3—Co1124.59 (14)
H2A—C2—H2B107.9C6—N3—H3C106.2
N2—C3—C2112.7 (2)Co1—N3—H3C106.2
N2—C3—H3A109.1C6—N3—H3D106.2
C2—C3—H3A109.1Co1—N3—H3D106.2
N2—C3—H3B109.1H3C—N3—H3D106.4
C2—C3—H3B109.1C4—N4—Co1122.49 (15)
H3A—C3—H3B107.8C4—N4—H4C106.7
N4—C4—C5112.6 (2)Co1—N4—H4C106.7
N4—C4—H4A109.1C4—N4—H4D106.7
C5—C4—H4A109.1Co1—N4—H4D106.7
N4—C4—H4B109.1H4C—N4—H4D106.6
C5—C4—H4B109.1C7—N5—Co1124.77 (16)
H4A—C4—H4B107.8C7—N5—H5C106.1
C6—C5—C4111.5 (2)Co1—N5—H5C106.1
C6—C5—H5A109.3C7—N5—H5D106.1
C4—C5—H5A109.3Co1—N5—H5D106.1
C6—C5—H5B109.3H5C—N5—H5D106.3
C4—C5—H5B109.3H1E—O1—H1F102 (3)
H5A—C5—H5B108.0N3—Co1—N593.88 (8)
N3—C6—C5112.6 (2)N3—Co1—N288.79 (8)
N3—C6—H6A109.1N5—Co1—N287.65 (8)
C5—C6—H6A109.1N3—Co1—N495.58 (8)
N3—C6—H6B109.1N5—Co1—N489.08 (9)
C5—C6—H6B109.1N2—Co1—N4174.72 (8)
H6A—C6—H6B107.8N3—Co1—N189.21 (8)
N5—C7—H7A109.5N5—Co1—N1176.46 (7)
N5—C7—H7B109.5N2—Co1—N194.16 (8)
H7A—C7—H7B109.5N4—Co1—N188.88 (8)
N5—C7—H7C109.5N3—Co1—Cl1177.67 (7)
H7A—C7—H7C109.5N5—Co1—Cl187.31 (6)
H7B—C7—H7C109.5N2—Co1—Cl189.26 (6)
C1—N1—Co1122.04 (16)N4—Co1—Cl186.43 (6)
C1—N1—H1C106.8N1—Co1—Cl189.67 (6)
N1—C1—C2—C3−69.3 (3)C7—N5—Co1—N497.9 (2)
C1—C2—C3—N269.8 (3)C7—N5—Co1—Cl1−175.7 (2)
N4—C4—C5—C672.5 (3)C3—N2—Co1—N3113.74 (19)
C4—C5—C6—N3−67.9 (3)C3—N2—Co1—N5−152.33 (19)
C2—C1—N1—Co148.1 (3)C3—N2—Co1—N124.62 (19)
C2—C3—N2—Co1−49.0 (3)C3—N2—Co1—Cl1−64.99 (18)
C5—C6—N3—Co135.5 (3)C4—N4—Co1—N311.6 (2)
C5—C4—N4—Co1−42.6 (3)C4—N4—Co1—N5−82.2 (2)
C6—N3—Co1—N581.2 (2)C4—N4—Co1—N1100.7 (2)
C6—N3—Co1—N2168.8 (2)C4—N4—Co1—Cl1−169.5 (2)
C6—N3—Co1—N4−8.2 (2)C1—N1—Co1—N3−113.12 (18)
C6—N3—Co1—N1−97.0 (2)C1—N1—Co1—N2−24.39 (19)
C7—N5—Co1—N32.3 (2)C1—N1—Co1—N4151.28 (19)
C7—N5—Co1—N2−86.3 (2)C1—N1—Co1—Cl164.84 (17)
D—H···AD—HH···AD···AD—H···A
N1—H1C···O10.902.122.960 (3)155
N1—H1D···Cl20.902.433.317 (2)170
N2—H2C···Cl3i0.902.573.462 (2)172
N2—H2D···Cl30.902.443.3196 (19)164
N3—H3C···O10.902.042.880 (3)155
N3—H3D···Cl30.902.503.3041 (18)149
N4—H4C···Cl3ii0.902.653.486 (2)155
N4—H4D···Cl20.902.453.348 (2)177
N5—H5C···Cl3i0.902.493.359 (2)162
N5—H5D···Cl3ii0.902.373.2649 (19)172
O1—H1E···Cl2iii0.82 (4)2.29 (4)3.093 (3)168 (4)
O1—H1F···Cl2iv0.87 (4)2.25 (4)3.112 (3)174 (3)
Table 1

Hydrogen-bond geometry (Å, °)

D—H⋯A D—HH⋯A D⋯A D—H⋯A
N1—H1C⋯O10.902.122.960 (3)155
N1—H1D⋯Cl20.902.433.317 (2)170
N2—H2C⋯Cl3i 0.902.573.462 (2)172
N2—H2D⋯Cl30.902.443.3196 (19)164
N3—H3C⋯O10.902.042.880 (3)155
N3—H3D⋯Cl30.902.503.3041 (18)149
N4—H4C⋯Cl3ii 0.902.653.486 (2)155
N4—H4D⋯Cl20.902.453.348 (2)177
N5—H5C⋯Cl3i 0.902.493.359 (2)162
N5—H5D⋯Cl3ii 0.902.373.2649 (19)172
O1—H1E⋯Cl2iii 0.82 (4)2.29 (4)3.093 (3)168 (4)
O1—H1F⋯Cl2iv 0.87 (4)2.25 (4)3.112 (3)174 (3)

Symmetry codes: (i) ; (ii) ; (iii) ; (iv) .

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