Literature DB >> 21579283

Tris(ethyl-enediamine)cobalt(II) sulfate.

Bunlawee Yotnoi¹, Athittaya Seeharaj, Yothin Chimupala, Apinpus Rujiwatra.

Abstract

The structure of the title compound, [Co(II)(C(2)H(8)N(2))(3)]SO(4), the cobalt example of [M(C(2)H(8)N(2))(3)]SO(4), is reported. The Co and S atoms are located at the 2d and 2c Wyckoff sites (point symmetry 32), respectively. The Co atom is coordinated by six N atoms of three chelating ethyl-enediamine mol-ecules generated from half of the ethyl-enediamine mol-ecule in the asymmetric unit. The O atoms of the sulfate anion are disordered mostly over two crystallographic sites. The third disorder site of O (site symmetry 3) has a site occupancy approaching zero. The H atoms of the ethyl-enediamine mol-ecules inter-act with the sulfate anions via inter-molecular N-H⋯O hydrogen-bonding inter-actions.

Entities: Chemical Disease Species

Year: 2010 PMID： 21579283 PMCID： PMC2979650 DOI： 10.1107/S1600536810016168

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

Related literature

For isostructural [M(C2H8N2)3]SO4 complexes, see: Haque et al. (1970 ▶); Cullen & Lingafelter (1970 ▶); Daniels et al. (1995 ▶); Lu (2009 ▶) for the nickel, copper, vanadium and manganese analogues, respectively.

Experimental

Crystal data

[Co(C2H8N2)3]SO4 M = 335.30 Trigonal, a = 8.9920 (2) Å c = 9.5927 (3) Å V = 671.71 (3) Å3 Z = 2 Mo Kα radiation μ = 1.45 mm−1 T = 298 K 0.48 × 0.22 × 0.20 mm

Data collection

Bruker SMART CCD area-detector diffractometer Absorption correction: multi-scan (SADABS; Sheldrick, 1996 ▶) T min = 0.543, T max = 0.760 3638 measured reflections 688 independent reflections 589 reflections with I > 2σ(I) R int = 0.027

Refinement

R[F 2 > 2σ(F 2)] = 0.028 wR(F 2) = 0.069 S = 1.06 688 reflections 47 parameters 16 restraints H-atom parameters constrained Δρmax = 0.25 e Å−3 Δρmin = −0.29 e Å−3 Data collection: SMART (Bruker, 2003 ▶); cell refinement: SAINT (Bruker, 2003 ▶); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶) and WinGX (Farrugia, 1999 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶) and WinGX (Farrugia, 1999 ▶); molecular graphics: DIAMOND (Brandenburg, 2006 ▶); software used to prepare material for publication: publCIF (Westrip, 2010 ▶). Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536810016168/tk2667sup1.cif Structure factors: contains datablocks I. DOI: 10.1107/S1600536810016168/tk2667Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report

[Co(C₂H₈N₂)₃]SO₄	D_x = 1.658 Mg m⁻³
M_r = 335.30	Mo Kα radiation, λ = 0.71073 Å
Trigonal, P31c	Cell parameters from 589 reflections
Hall symbol: -P 3 2c	θ = 2.6–31.0°
a = 8.9920 (2) Å	µ = 1.45 mm⁻¹
c = 9.5927 (3) Å	T = 298 K
V = 671.71 (3) Å³	Block, orange
Z = 2	0.48 × 0.22 × 0.20 mm
F(000) = 354

Bruker SMART CCD area-detector diffractometer	688 independent reflections
Radiation source: fine-focus sealed tube	589 reflections with I > 2σ(I)
graphite	R_int = 0.027
? scan	θ_max = 31.0°, θ_min = 2.6°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	h = −8→10
T_min = 0.543, T_max = 0.760	k = −11→11
3638 measured reflections	l = −11→13

Refinement on F²	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F² > 2σ(F²)] = 0.028	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.069	H-atom parameters constrained
S = 1.06	w = 1/[σ²(F_o²) + (0.0354P)² + 0.1217P] where P = (F_o² + 2F_c²)/3
688 reflections	(Δ/σ)_max < 0.001
47 parameters	Δρ_max = 0.25 e Å⁻³
16 restraints	Δρ_min = −0.29 e Å⁻³

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds 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.

	x	y	z	U_iso*/U_eq	Occ. (<1)
Co1	0.6667	0.3333	0.2500	0.02175 (16)
N1	0.68784 (18)	0.54599 (18)	0.12760 (13)	0.0332 (3)
H1A	0.6936	0.5265	0.0363	0.040*
H1B	0.5954	0.5579	0.1418	0.040*
S1	0.3333	0.6667	0.2500	0.0240 (2)
C1	0.8446 (2)	0.7024 (2)	0.17145 (19)	0.0388 (4)
H1C	0.8405	0.8031	0.1409	0.047*
H1D	0.9444	0.7056	0.1297	0.047*
O1	0.3029 (19)	0.5088 (9)	0.1852 (8)	0.096 (3)	0.319 (8)
O2	0.339 (2)	0.7851 (9)	0.1475 (6)	0.096 (4)	0.316 (9)
O3	0.3333	0.6667	0.1059 (16)	0.086 (8)	0.094 (10)

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Co1	0.0226 (2)	0.0226 (2)	0.0201 (2)	0.01129 (10)	0.000	0.000
N1	0.0410 (8)	0.0330 (7)	0.0283 (7)	0.0204 (6)	−0.0033 (5)	0.0031 (5)
S1	0.0243 (3)	0.0243 (3)	0.0233 (4)	0.01215 (14)	0.000	0.000
C1	0.0445 (10)	0.0267 (8)	0.0413 (9)	0.0147 (7)	0.0058 (7)	0.0076 (6)
O1	0.185 (9)	0.051 (4)	0.063 (4)	0.069 (5)	−0.012 (5)	−0.016 (3)
O2	0.194 (12)	0.055 (4)	0.044 (3)	0.067 (5)	−0.012 (4)	0.012 (3)
O3	0.118 (11)	0.118 (11)	0.021 (11)	0.059 (5)	0.000	0.000

Co1—N1ⁱ	2.1696 (13)	S1—O2^vi	1.431 (5)
Co1—N1ⁱⁱ	2.1696 (13)	S1—O2^v	1.431 (5)
Co1—N1ⁱⁱⁱ	2.1696 (13)	S1—O2^vii	1.431 (5)
Co1—N1^iv	2.1696 (13)	S1—O2^viii	1.431 (5)
Co1—N1	2.1696 (13)	S1—O2^ix	1.431 (5)
Co1—N1^v	2.1696 (13)	S1—O1^ix	1.445 (5)
N1—C1	1.469 (2)	S1—O1^viii	1.445 (5)
N1—H1A	0.9000	S1—O1^vi	1.445 (5)
N1—H1B	0.9000	S1—O1^vii	1.445 (5)
S1—O3	1.382 (16)	C1—C1^iv	1.512 (4)
S1—O3^v	1.382 (16)	C1—H1C	0.9700
S1—O2	1.431 (5)	C1—H1D	0.9700

N1ⁱ—Co1—N1ⁱⁱ	80.49 (7)	O2^viii—S1—O1^viii	110.7 (4)
N1ⁱ—Co1—N1ⁱⁱⁱ	93.48 (5)	O2^ix—S1—O1^viii	138.0 (11)
N1ⁱⁱ—Co1—N1ⁱⁱⁱ	93.17 (8)	O1^ix—S1—O1^viii	63.4 (8)
N1ⁱ—Co1—N1^iv	93.17 (8)	O3—S1—O1^vi	64.5 (3)
N1ⁱⁱ—Co1—N1^iv	93.48 (5)	O3^v—S1—O1^vi	115.5 (3)
N1ⁱⁱⁱ—Co1—N1^iv	171.28 (7)	O2—S1—O1^vi	57.2 (5)
N1ⁱ—Co1—N1	93.48 (5)	O2^vi—S1—O1^vi	110.7 (4)
N1ⁱⁱ—Co1—N1	171.28 (8)	O2^v—S1—O1^vi	138.0 (11)
N1ⁱⁱⁱ—Co1—N1	93.48 (5)	O2^vii—S1—O1^vi	69.9 (6)
N1^iv—Co1—N1	80.49 (7)	O2^viii—S1—O1^vi	45.7 (4)
N1ⁱ—Co1—N1^v	171.28 (8)	O2^ix—S1—O1^vi	119.2 (10)
N1ⁱⁱ—Co1—N1^v	93.48 (5)	O1^ix—S1—O1^vi	93.3 (11)
N1ⁱⁱⁱ—Co1—N1^v	80.49 (7)	O1^viii—S1—O1^vi	102.9 (4)
N1^iv—Co1—N1^v	93.48 (5)	O3—S1—O1^vii	115.5 (3)
N1—Co1—N1^v	93.17 (8)	O3^v—S1—O1^vii	64.5 (3)
C1—N1—Co1	107.94 (10)	O2—S1—O1^vii	138.0 (11)
C1—N1—H1A	110.1	O2^vi—S1—O1^vii	69.9 (6)
Co1—N1—H1A	110.1	O2^v—S1—O1^vii	57.2 (5)
C1—N1—H1B	110.1	O2^vii—S1—O1^vii	110.7 (4)
Co1—N1—H1B	110.1	O2^viii—S1—O1^vii	119.2 (10)
H1A—N1—H1B	108.4	O2^ix—S1—O1^vii	45.7 (4)
O3—S1—O3^v	180.000 (3)	O1^ix—S1—O1^vii	102.9 (4)
O3—S1—O2	46.6 (3)	O1^viii—S1—O1^vii	93.3 (11)
O3^v—S1—O2	133.4 (3)	O1^vi—S1—O1^vii	161.1 (12)
O3—S1—O2^vi	46.6 (3)	N1—C1—C1^iv	108.84 (12)
O3^v—S1—O2^vi	133.4 (3)	N1—C1—H1C	109.9
O2—S1—O2^vi	78.0 (5)	C1^iv—C1—H1C	109.9
O3—S1—O2^v	133.4 (3)	N1—C1—H1D	109.9
O3^v—S1—O2^v	46.6 (3)	C1^iv—C1—H1D	109.9
O2—S1—O2^v	104.4 (11)	H1C—C1—H1D	108.3
O2^vi—S1—O2^v	99.7 (7)	O2^vi—O1—O2^viii	91.9 (8)
O3—S1—O2^vii	133.4 (3)	O2^vi—O1—S1	66.5 (5)
O3^v—S1—O2^vii	46.6 (3)	O2^viii—O1—S1	60.9 (3)
O2—S1—O2^vii	99.7 (7)	O2^vi—O1—O1^vii	75.7 (11)
O2^vi—S1—O2^vii	176.3 (13)	O2^viii—O1—O1^vii	117.8 (4)
O2^v—S1—O2^vii	78.0 (5)	S1—O1—O1^vii	58.3 (4)
O3—S1—O2^viii	46.6 (3)	O2^vi—O1—O2^ix	108.3 (7)
O3^v—S1—O2^viii	133.4 (3)	O2^viii—O1—O2^ix	92.2 (8)
O2—S1—O2^viii	78.0 (5)	S1—O1—O2^ix	54.6 (4)
O2^vi—S1—O2^viii	78.0 (5)	O1^viii—O2—O1^vi	129.8 (7)
O2^v—S1—O2^viii	176.3 (13)	O1^viii—O2—S1	67.8 (4)
O2^vii—S1—O2^viii	104.4 (11)	O1^vi—O2—S1	61.9 (4)
O3—S1—O2^ix	133.4 (3)	O1^viii—O2—O1^ix	63.3 (12)
O3^v—S1—O2^ix	46.6 (3)	O1^vi—O2—O1^ix	87.5 (9)
O2—S1—O2^ix	176.3 (13)	S1—O2—O1^ix	55.5 (3)
O2^vi—S1—O2^ix	104.4 (11)	O1^viii—O2—O2^vi	49.8 (6)
O2^v—S1—O2^ix	78.0 (5)	O1^vi—O2—O2^vi	95.3 (5)
O2^vii—S1—O2^ix	78.0 (5)	S1—O2—O2^vi	51.0 (2)
O2^viii—S1—O2^ix	99.7 (7)	O1^ix—O2—O2^vi	91.9 (8)
O3—S1—O1^ix	115.5 (3)	O1^viii—O2—O2^viii	106.1 (5)
O3^v—S1—O1^ix	64.5 (3)	S1—O2—O2^viii	51.0 (2)
O2—S1—O1^ix	69.9 (6)	O1^ix—O2—O2^viii	102.2 (4)
O2^vi—S1—O1^ix	119.2 (10)	O2^vi—O2—O2^viii	60.000 (1)
O2^v—S1—O1^ix	45.7 (4)	O2^vi—O3—O2^viii	107.9 (8)
O2^vii—S1—O1^ix	57.2 (5)	O2^vi—O3—S1	69.0 (8)
O2^viii—S1—O1^ix	138.0 (11)	O2^viii—O3—S1	69.0 (8)
O2^ix—S1—O1^ix	110.7 (4)	O2^vi—O3—O1^viii	61.1 (6)
O3—S1—O1^viii	64.5 (3)	O2^viii—O3—O1^viii	128.2 (13)
O3^v—S1—O1^viii	115.5 (3)	S1—O3—O1^viii	59.8 (5)
O2—S1—O1^viii	45.7 (4)	O2^vi—O3—O1^vi	128.2 (13)
O2^vi—S1—O1^viii	57.2 (5)	O2^viii—O3—O1^vi	47.4 (6)
O2^v—S1—O1^viii	69.9 (6)	S1—O3—O1^vi	59.8 (5)
O2^vii—S1—O1^viii	119.2 (10)	O1^viii—O3—O1^vi	96.9 (7)

D—H···A	D—H	H···A	D···A	D—H···A
N1—H1A···O3^x	0.90	2.13	2.889 (12)	142
N1—H1A···O1^x	0.90	2.15	3.049 (7)	176
N1—H1A···O2^xi	0.90	2.22	3.054 (8)	155
N1—H1A···O2^xii	0.90	2.32	3.104 (11)	145
N1—H1B···O2^viii	0.90	1.98	2.843 (6)	161
N1—H1B···O1	0.90	2.48	3.353 (14)	165
N1—H1B···O1^v	0.90	2.52	3.256 (10)	139

Table 1

Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
N1—H1A⋯O3ⁱ	0.90	2.13	2.889 (12)	142
N1—H1A⋯O1ⁱ	0.90	2.15	3.049 (7)	176
N1—H1A⋯O2ⁱⁱ	0.90	2.22	3.054 (8)	155
N1—H1A⋯O2ⁱⁱⁱ	0.90	2.32	3.104 (11)	145
N1—H1B⋯O2^iv	0.90	1.98	2.843 (6)	161
N1—H1B⋯O1	0.90	2.48	3.353 (14)	165
N1—H1B⋯O1^v	0.90	2.52	3.256 (10)	139

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

2 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. Tris(ethyl-enediamine)manganese(II) sulfate.

Authors: Jing Lu
Journal: Acta Crystallogr Sect E Struct Rep Online Date: 2009-09-09

2 in total