Download citation
Download citation
link to html
In the title complex, [Ni(C2H8N2)2](NO3)2, the two ethyl­enediamine groups, (en), and the nitrate anions are related by an inversion center at the Ni atom. The coordination about the Ni atom can be described as a tetragonally distorted octahedron with four equatorial sites occupied by the N atoms of the (en) groups and the two axial sites by the nitrate anions through a `semi-coordinating' Ni...O interaction of 2.5539 (15) Å. The remaining O atoms of the nitrate groups participate in N—H...O hydrogen-bonding interactions with the (en) ligand.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536804032052/ac6145sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536804032052/ac6145Isup2.hkl
Contains datablock I

Key indicators

  • Single-crystal X-ray study
  • T = 150 K
  • Mean [sigma](C-C) = 0.003 Å
  • R factor = 0.031
  • wR factor = 0.091
  • Data-to-parameter ratio = 13.0

checkCIF/PLATON results

No syntax errors found



Alert level B PLAT232_ALERT_2_B Hirshfeld Test Diff (M-X) Ni - O2 .. 10.52 su PLAT232_ALERT_2_B Hirshfeld Test Diff (M-X) Ni - N1 .. 13.87 su PLAT232_ALERT_2_B Hirshfeld Test Diff (M-X) Ni - N2 .. 12.52 su
Alert level C PLAT029_ALERT_3_C _diffrn_measured_fraction_theta_full Low ....... 0.97 PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for O2 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for Ni PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 3 N1 -NI -N1 -C3 82.00 7.00 3.655 1.555 1.555 1.555 PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 4 N2 -NI -N2 -C4 -35.00 7.00 3.655 1.555 1.555 1.555
0 ALERT level A = In general: serious problem 3 ALERT level B = Potentially serious problem 6 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 1 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 5 ALERT type 2 Indicator that the structure model may be wrong or deficient 1 ALERT type 3 Indicator that the structure quality may be low 2 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: SMART (Bruker, 2002); cell refinement: SAINT (Bruker, 2002); data reduction: SAINT; program(s) used to solve structure: SHELXTL (Sheldrick, 2003); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.

Bis(ethylenediamine)nickel(II) dinitrate top
Crystal data top
[Ni(C2H8N2)2](NO3)2F(000) = 316
Mr = 302.94Dx = 1.681 Mg m3
Monoclinic, P21/cCu Kα radiation, λ = 1.54178 Å
Hall symbol: -P 2ybcCell parameters from 2387 reflections
a = 8.2382 (2) Åθ = 4.4–65.0°
b = 10.0125 (3) ŵ = 2.67 mm1
c = 7.8277 (2) ÅT = 150 K
β = 111.998 (1)°Plate, pale purple
V = 598.66 (3) Å30.29 × 0.11 × 0.01 mm
Z = 2
Data collection top
Bruker SMART 6000 CCD
diffractometer
926 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tubeRint = 0.026
ω scansθmax = 67.0°, θmin = 5.8°
Absorption correction: multi-scan
(SADABS; Sheldrick, 2003)
h = 98
Tmin = 0.512, Tmax = 0.974k = 119
3389 measured reflectionsl = 98
1027 independent reflections
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)] = 0.031Hydrogen site location: mixed
wR(F2) = 0.092H-atom parameters constrained
S = 1.08 w = 1/[σ2(Fo2) + (0.0595P)2 + 0.1767P]
where P = (Fo2 + 2Fc2)/3
1027 reflections(Δ/σ)max < 0.001
79 parametersΔρmax = 0.38 e Å3
0 restraintsΔρmin = 0.27 e Å3
Special details top

Experimental. The crystal was mounted in a Cryo-loop with Paratone-N.

The final unit cell is obtained from the refinement of the XYZ weighted centroids of reflections above 20 σ(I).

Note that the absorption correction parameters Tmin and Tmax also reflect beam corrections, etc. As a result, the numerical values for Tmin and Tmax may differ from expected values based solely on absorption effects and crystal size.

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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Ni0.50000.00000.00000.0172 (2)
N10.6621 (2)0.15537 (18)0.0206 (3)0.0328 (4)
H1A0.68600.16200.08490.039*
H1B0.61010.23360.03500.039*
N20.7099 (2)0.08746 (18)0.1871 (2)0.0298 (4)
H2A0.70120.08590.30090.036*
H2B0.71680.17510.15510.036*
C30.8260 (3)0.1333 (2)0.1815 (4)0.0439 (6)
H3A0.81170.16380.29540.053*
H3B0.92280.18460.16700.053*
C40.8675 (4)0.0141 (2)0.1942 (4)0.0383 (6)
H4A0.90100.04160.09050.046*
H4B0.96630.03380.31100.046*
N30.3284 (2)0.05798 (19)0.3331 (2)0.0289 (4)
O10.2690 (2)0.12956 (16)0.4279 (2)0.0390 (4)
O20.4085 (2)0.11111 (16)0.2437 (2)0.0400 (4)
O30.3045 (2)0.06558 (16)0.3278 (2)0.0408 (4)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ni0.0233 (3)0.0102 (3)0.0182 (3)0.00025 (15)0.0080 (2)0.00177 (14)
N10.0416 (11)0.0208 (9)0.0370 (10)0.0001 (8)0.0160 (8)0.0003 (7)
N20.0377 (10)0.0249 (9)0.0274 (9)0.0021 (7)0.0129 (7)0.0008 (7)
C30.0402 (14)0.0293 (13)0.0540 (15)0.0053 (10)0.0083 (11)0.0047 (11)
C40.0362 (13)0.0319 (13)0.0441 (14)0.0015 (9)0.0119 (11)0.0009 (9)
N30.0377 (11)0.0230 (10)0.0245 (9)0.0006 (8)0.0101 (8)0.0008 (7)
O10.0578 (11)0.0300 (9)0.0368 (9)0.0050 (7)0.0264 (8)0.0006 (7)
O20.0584 (11)0.0305 (9)0.0420 (9)0.0067 (7)0.0312 (8)0.0036 (7)
O30.0599 (11)0.0210 (9)0.0448 (10)0.0020 (8)0.0235 (8)0.0015 (7)
Geometric parameters (Å, º) top
Ni—N22.0015 (18)N2—H2B0.9200
Ni—N2i2.0015 (18)C3—C41.510 (3)
Ni—N12.0171 (18)C3—H3A0.9900
Ni—N1i2.0171 (18)C3—H3B0.9900
N1—C31.478 (3)C4—H4A0.9900
N1—H1A0.9200C4—H4B0.9900
N1—H1B0.9200N3—O21.247 (2)
N2—C41.474 (3)N3—O31.251 (3)
N2—H2A0.9200N3—O11.255 (2)
N2—Ni—N2i180.0H2A—N2—H2B108.4
N2—Ni—N185.08 (7)N1—C3—C4108.30 (19)
N2i—Ni—N194.92 (7)N1—C3—H3A110.0
N2—Ni—N1i94.92 (7)C4—C3—H3A110.0
N2i—Ni—N1i85.08 (7)N1—C3—H3B110.0
N1—Ni—N1i180.0C4—C3—H3B110.0
C3—N1—Ni108.60 (14)H3A—C3—H3B108.4
C3—N1—H1A110.0N2—C4—C3108.1 (2)
Ni—N1—H1A110.0N2—C4—H4A110.1
C3—N1—H1B110.0C3—C4—H4A110.1
Ni—N1—H1B110.0N2—C4—H4B110.1
H1A—N1—H1B108.3C3—C4—H4B110.1
C4—N2—Ni108.47 (14)H4A—C4—H4B108.4
C4—N2—H2A110.0O2—N3—O3120.85 (17)
Ni—N2—H2A110.0O2—N3—O1119.59 (18)
C4—N2—H2B110.0O3—N3—O1119.55 (16)
Ni—N2—H2B110.0
N2—Ni—N1—C311.64 (15)N1i—Ni—N2—C4163.78 (15)
N2i—Ni—N1—C3168.36 (15)Ni—N1—C3—C436.6 (2)
N1i—Ni—N1—C382 (7)Ni—N2—C4—C340.4 (2)
N2i—Ni—N2—C435 (7)N1—C3—C4—N251.2 (3)
N1—Ni—N2—C416.22 (15)
Symmetry code: (i) x+1, y, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N1—H1A···O3i0.922.162.980 (3)148
N1—H1B···O3ii0.922.263.008 (2)138
N2—H2A···O1iii0.922.092.983 (2)163
N2—H2B···O1iv0.922.082.998 (2)178
Symmetry codes: (i) x+1, y, z; (ii) x+1, y+1/2, z+1/2; (iii) x+1, y, z+1; (iv) x+1, y1/2, z+1/2.
 

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