Download citation
Download citation
link to html
The title compound, [Ni{N(CH2CH2OH)3}2](CH3COO)2, was prepared and the structure determined. It is isostructural with the copper(II) analogue.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270100004819/qa0257sup1.cif
Contains datablocks I, default

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108270100004819/qa0257Isup2.hkl
Contains datablock I

CCDC reference: 145627

Comment top

The Ni2+ cation is coordinated by two molecules of triethanolamine,forming an octahedron. This octahedron shows only a slight distortion compared with the Jahn–Teller distortion of Cu2+ in the isostructural compound [Cu{N(CH2CH2OH)3}2](CH3COO)2 (Krabbes et al., 1999). Acetate ions are linked by hydrogen bonds to the triethanolamine hydroxyl groups of the [Ni{N(CH2CH2OH)3}2]2+ complex cation. Each acetate ion is linked by two hydrogen bonds to the coordinated hydroxyl groups of the complex cation and by a third hydrogen bond to the free hydroxyl group of a second complex cation species. This causes the formation of chains along the a axis. Table 1 contains the interatomic distances and angles of the title compound, (I). The IR spectrum of the complex shows absorption bands of associated hydroxyl groups at 3260 and 3035 cm-1. Between 3000 and 2400 cm-1, the typical absorption bands of O—H···O-chelates are observed. Valence vibrations of carboxyl groups occur at 1545 (νas) and 1415 cm-1 (νs).

Experimental top

The synthesis of the title compound was carried out by dissolving nickel(II) acetate tetrahydrate in a tenfold excess of triethanolamine at 423 K. Polycrystalline bis(triethanolamine)nickel(II) acetate precipitated when the solution was cooled down. After removing the excess of triethanolamine the product was washed with acetone. Single crystals of bis(triethanolamine)nickel(II) acetate were obtained by fractional crystallization from a triethanolamine solution. The IR spectrum was recorded using a potassium bromide matrix on a Perkin Elmer FT–IR 2000 spectrometer.

Computing details top

Data collection: CAD-4 Software (Enraf-Nonius, 1989); cell refinement: CAD-4 Software; data reduction: HELENA (Spek, 1992); program(s) used to solve structure: SHELXS86 (Sheldrick, 1990); program(s) used to refine structure: SHELXL93 (Sheldrick, 1993); molecular graphics: DIAMOND (Branderburg, 1996); software used to prepare material for publication: DIAMOND.

Bis(triethanolamine)nickel(II) acetate top
Crystal data top
[Ni(C6H15NO3)2](C2H3O2)2Dx = 1.439 Mg m3
Mr = 475.18Melting point: not measured K
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
a = 9.123 (1) ÅCell parameters from 25 reflections
b = 13.219 (2) Åθ = 12.4–18.7°
c = 9.820 (1) ŵ = 0.94 mm1
β = 112.17 (6)°T = 296 K
V = 1096.7 (2) Å3Prism, clear light blue
Z = 20.40 × 0.40 × 0.40 mm
F(000) = 508
Data collection top
Enraf-Nonius CAD-4
diffractometer
Rint = 0.017
Radiation source: fine-focus sealed tubeθmax = 26.9°, θmin = 2.4°
Graphite monochromatorh = 011
ω–2θ scansk = 016
2524 measured reflectionsl = 1211
2379 independent reflections3 standard reflections every 250 reflections
2048 reflections with I > 2σ(I) intensity decay: none
Refinement top
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) = 0.077H-atom parameters constrained
S = 0.98Calculated w = 1/[σ2(Fo2) + (0.0492P)2 + 0.4638P]
where P = (Fo2 + 2Fc2)/3
2379 reflections(Δ/σ)max < 0.001
136 parametersΔρmax = 0.51 e Å3
0 restraintsΔρmin = 0.27 e Å3
Crystal data top
[Ni(C6H15NO3)2](C2H3O2)2V = 1096.7 (2) Å3
Mr = 475.18Z = 2
Monoclinic, P21/cMo Kα radiation
a = 9.123 (1) ŵ = 0.94 mm1
b = 13.219 (2) ÅT = 296 K
c = 9.820 (1) Å0.40 × 0.40 × 0.40 mm
β = 112.17 (6)°
Data collection top
Enraf-Nonius CAD-4
diffractometer
Rint = 0.017
2524 measured reflections3 standard reflections every 250 reflections
2379 independent reflections intensity decay: none
2048 reflections with I > 2σ(I)
Refinement top
R[F2 > 2σ(F2)] = 0.0300 restraints
wR(F2) = 0.077H-atom parameters constrained
S = 0.98Δρmax = 0.51 e Å3
2379 reflectionsΔρmin = 0.27 e Å3
136 parameters
Special details top

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 on F2 for ALL reflections except for 0 with very negative F2 or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F2, conventional R-factors R are based on F, with F set to zero for negative F2. The observed criterion of F2 > σ(F2) is used only for calculating R-factor-obs 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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Ni10.00000.00000.00000.02587 (10)
O10.2945 (2)0.08394 (12)0.34039 (15)0.0516 (4)
H10.37660.11430.29400
O20.21979 (15)0.00995 (9)0.17099 (13)0.0344 (3)
H20.27570.05480.15870
O30.01338 (14)0.15305 (9)0.04444 (14)0.0342 (3)
H30.07010.18460.01700
O40.4124 (2)0.84668 (11)0.1654 (2)0.0549 (4)
O50.2379 (2)0.74044 (11)0.0168 (2)0.0580 (4)
N10.0782 (2)0.04235 (11)0.16804 (14)0.0302 (3)
C10.2085 (2)0.0224 (2)0.3124 (2)0.0422 (4)
H1A0.28340.02220.38340
H1B0.23480.09150.34580
C20.0422 (2)0.00191 (14)0.3017 (2)0.0391 (4)
H2A0.02720.024270.38780
H2B0.02860.074730.30010
C30.2384 (2)0.00026 (13)0.1397 (2)0.0381 (4)
H3A0.31500.041780.06500
H3B0.24320.066870.09840
C40.2912 (3)0.0078 (2)0.2693 (2)0.0462 (5)
H4A0.22060.05410.34090
H4B0.39640.03720.23460
C50.0768 (2)0.15532 (13)0.1723 (2)0.0363 (4)
H5A0.02690.179080.23650
H5B0.15380.179290.21110
C60.1162 (2)0.19649 (13)0.0191 (2)0.0382 (4)
H6A0.22530.180700.04140
H6B0.10430.269480.02320
C70.3762 (2)0.76707 (14)0.0914 (2)0.0402 (4)
C80.5091 (3)0.6992 (2)0.0898 (3)0.0572 (6)
H8A0.60890.72790.15110
H8B0.50500.69320.00910
H8C0.49780.63350.12620
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ni10.0305 (2)0.0236 (2)0.0225 (2)0.00088 (10)0.00886 (11)0.00019 (10)
O10.0476 (8)0.0707 (10)0.0385 (7)0.0038 (7)0.0185 (6)0.0085 (7)
O20.0351 (6)0.0365 (7)0.0292 (6)0.0019 (5)0.0093 (5)0.0005 (5)
O30.0392 (6)0.0273 (6)0.0364 (6)0.0015 (5)0.0145 (5)0.0022 (5)
O40.0431 (8)0.0475 (8)0.0633 (9)0.0062 (6)0.0081 (7)0.0122 (7)
O50.0369 (7)0.0445 (8)0.0835 (11)0.0044 (6)0.0126 (7)0.0126 (7)
N10.0345 (7)0.0287 (7)0.0266 (6)0.0012 (6)0.0105 (6)0.0002 (5)
C10.0410 (10)0.0524 (11)0.0264 (8)0.0084 (8)0.0050 (7)0.0019 (7)
C20.0464 (10)0.0448 (10)0.0254 (8)0.0083 (8)0.0128 (7)0.0042 (7)
C30.0400 (9)0.0406 (10)0.0355 (9)0.0059 (7)0.0164 (8)0.0040 (7)
C40.0465 (11)0.0544 (12)0.0428 (10)0.0017 (9)0.0228 (9)0.0040 (8)
C50.0416 (9)0.0308 (8)0.0368 (9)0.0025 (7)0.0151 (7)0.0057 (7)
C60.0415 (10)0.0293 (8)0.0432 (10)0.0056 (7)0.0153 (8)0.0033 (7)
C70.0385 (9)0.0361 (9)0.0459 (10)0.0039 (7)0.0159 (8)0.0037 (8)
C80.0399 (11)0.0516 (12)0.078 (2)0.0046 (9)0.0203 (10)0.0091 (11)
Geometric parameters (Å, º) top
Ni1—O3i2.0636 (12)N1—C21.477 (2)
Ni1—O2i2.078 (2)N1—C31.489 (2)
Ni1—N1i2.1055 (14)N1—C5i1.494 (2)
Ni1—N12.1055 (14)C1—C21.515 (3)
O1—C41.405 (2)C3—C41.525 (3)
O2—C11.440 (2)C5—N1i1.494 (2)
O3—C61.429 (2)C5—C61.510 (2)
O4—C71.251 (2)C7—C81.513 (3)
O5—C71.247 (2)
O3i—Ni1—O2i85.93 (5)C5i—N1—Ni1106.61 (10)
O3i—Ni1—N1i96.05 (5)O2—C1—C2110.1 (2)
O2i—Ni1—N1i81.88 (5)N1—C2—C1111.5 (2)
O3i—Ni1—N183.95 (5)N1—C3—C4117.9 (2)
O2i—Ni1—N198.12 (5)O1—C4—C3115.2 (2)
N1i—Ni1—N1180.0N1i—C5—C6109.64 (14)
C2—N1—C3111.49 (15)O3—C6—C5109.98 (14)
C2—N1—C5i112.05 (13)O5—C7—O4124.4 (2)
C3—N1—C5i112.09 (13)O5—C7—C8117.6 (2)
C2—N1—Ni1103.46 (10)O4—C7—C8117.9 (2)
C3—N1—Ni1110.68 (11)
O3i—Ni1—N1—C2125.78 (11)C3—N1—C2—C1167.35 (15)
O2i—Ni1—N1—C2149.22 (11)C5i—N1—C2—C166.1 (2)
N1i—Ni1—N1—C2103 (3)Ni1—N1—C2—C148.4 (2)
O3i—Ni1—N1—C3114.68 (12)O2—C1—C2—N143.2 (2)
O2i—Ni1—N1—C329.68 (12)C2—N1—C3—C445.4 (2)
N1i—Ni1—N1—C317 (3)C5i—N1—C3—C481.1 (2)
O3i—Ni1—N1—C5i7.47 (10)Ni1—N1—C3—C4160.03 (13)
O2i—Ni1—N1—C5i92.47 (10)N1—C3—C4—O159.0 (2)
N1i—Ni1—N1—C5i139 (3)N1i—C5—C6—O353.3 (2)
Symmetry code: (i) x, y, z.

Experimental details

Crystal data
Chemical formula[Ni(C6H15NO3)2](C2H3O2)2
Mr475.18
Crystal system, space groupMonoclinic, P21/c
Temperature (K)296
a, b, c (Å)9.123 (1), 13.219 (2), 9.820 (1)
β (°) 112.17 (6)
V3)1096.7 (2)
Z2
Radiation typeMo Kα
µ (mm1)0.94
Crystal size (mm)0.40 × 0.40 × 0.40
Data collection
DiffractometerEnraf-Nonius CAD-4
diffractometer
Absorption correction
No. of measured, independent and
observed [I > 2σ(I)] reflections
2524, 2379, 2048
Rint0.017
(sin θ/λ)max1)0.637
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.030, 0.077, 0.98
No. of reflections2379
No. of parameters136
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)0.51, 0.27

Computer programs: CAD-4 Software (Enraf-Nonius, 1989), CAD-4 Software, HELENA (Spek, 1992), SHELXS86 (Sheldrick, 1990), SHELXL93 (Sheldrick, 1993), DIAMOND (Branderburg, 1996), DIAMOND.

Selected geometric parameters (Å, º) top
Ni1—O3i2.0636 (12)Ni1—N1i2.1055 (14)
Ni1—O2i2.078 (2)
O3i—Ni1—O2i85.93 (5)O3i—Ni1—N183.95 (5)
O2i—Ni1—N1i81.88 (5)
Symmetry code: (i) x, y, z.
 

Follow Acta Cryst. C
Sign up for e-alerts
Follow Acta Cryst. on Twitter
Follow us on facebook
Sign up for RSS feeds