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The title compound, [NiBr2(C4H12N2)2], is a mol­ecular nickel(II) complex. The nickel(II) center is pseudo-octa­hedral six-coordinate with a trans geometry and is located on an inversion center. The mol­ecules exhibit limited hydrogen bonding between the axial bromide ions and the secondary amine H atoms (each halide inter­acts with two H atoms) of adjacent mol­ecules.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806033769/bv2025sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536806033769/bv2025Isup2.hkl
Contains datablock I

CCDC reference: 620706

Key indicators

  • Single-crystal X-ray study
  • T = 295 K
  • Mean [sigma](C-C) = 0.005 Å
  • R factor = 0.072
  • wR factor = 0.147
  • Data-to-parameter ratio = 18.0

checkCIF/PLATON results

No syntax errors found



Alert level A PLAT222_ALERT_3_A Large Non-Solvent H Ueq(max)/Ueq(min) ... 6.40 Ratio
Author Response: see _publ_section_exptl_refinement. One methyl group is disordered, so one set of hydrogen atoms has a small Ueq producing a small Ueq(min).

Alert level C PLAT029_ALERT_3_C _diffrn_measured_fraction_theta_full Low ....... 0.97 PLAT245_ALERT_2_C U(iso) H10 Smaller than U(eq) C3 by ... 0.04 AngSq PLAT245_ALERT_2_C U(iso) H11 Smaller than U(eq) C3 by ... 0.04 AngSq PLAT245_ALERT_2_C U(iso) H12 Smaller than U(eq) C3 by ... 0.04 AngSq PLAT420_ALERT_2_C D-H Without Acceptor N1 - H2 ... ?
1 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 5 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 4 ALERT type 2 Indicator that the structure model may be wrong or deficient 2 ALERT type 3 Indicator that the structure quality may be low 0 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check

Computing details top

Data collection: CAD-4 EXPRESS (Enraf–Nonius, 1994); cell refinement: CAD-4 EXPRESS; data reduction: maXus (Mackay et al., 1999); program(s) used to solve structure: SIR92 (Altomare et al., 1993); program(s) used to refine structure: TEXSAN for Window (Molecular Structure Corporation, 1999); software used to prepare material for publication: TEXSAN for Windows.

trans-Dibromobis(N,N'-dimethylethane-1,2-diamine-κ2N,N')nickel(II) top
Crystal data top
[NiBr2(C4H12N2)2]F(000) = 396.00
Mr = 394.81Dx = 1.836 Mg m3
Monoclinic, P21/cCu Kα radiation, λ = 1.5418 Å
Hall symbol: -P 2ybcCell parameters from 25 reflections
a = 7.8731 (5) Åθ = 23.5–46.8°
b = 8.6501 (4) ŵ = 8.35 mm1
c = 10.6902 (7) ÅT = 295 K
β = 101.206 (5)°Fragment, blue
V = 714.16 (7) Å30.22 × 0.15 × 0.10 mm
Z = 2
Data collection top
Enraf–Nonius CAD-4
diffractometer
1277 reflections with I > 3.00σ(I)
Radiation source: fine-focus sealed tubeRint = 0.070
Graphite monochromatorθmax = 75.1°, θmin = 5.7°
ω–2θ scansh = 99
Absorption correction: ψ scan
(North et al, 1968)
k = 1010
Tmin = 0.269, Tmax = 0.434l = 1313
4858 measured reflections3 standard reflections every 120 min
1427 independent reflections intensity decay: 1.5%
Refinement top
Refinement on F20 restraints
Least-squares matrix: full5 constraints
R[F2 > 2σ(F2)] = 0.072H-atom parameters constrained
wR(F2) = 0.147Weighting scheme based on measured s.u.'s w = 1/[σ2(Fo) + 0.0036|Fo|2]
S = 1.03(Δ/σ)max = 0.001
1277 reflectionsΔρmax = 0.88 e Å3
71 parametersΔρmin = 1.02 e Å3
Special details top

Experimental. 1H NMR (300 MHz, D2O): 50, 70, 84, 89, 112, 115.

Refinement. Refinement of F2. The weighted R-factor wR and goodness of fit are based on F2, conventional R-factors R are based on F. R-factors based on F2 are statistically about twice as large as those based on F.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Br10.36287 (5)0.50734 (4)0.70969 (3)0.0408 (2)
Ni10.50000.50000.50000.0266 (3)
N10.3228 (3)0.3254 (3)0.4203 (2)0.0324 (5)
N20.3140 (3)0.6530 (3)0.3946 (2)0.0360 (5)
C10.1594 (3)0.4077 (4)0.3705 (3)0.0495 (7)
C20.1953 (4)0.5531 (5)0.3046 (3)0.0535 (9)
C30.2898 (4)0.1928 (4)0.4967 (3)0.0458 (7)
C40.2235 (4)0.7613 (4)0.4638 (3)0.0500 (8)
H10.37470.71430.34400.043*
H20.36300.28530.34860.039*
H30.16390.83560.40610.060*
H40.30500.81210.52770.060*
H50.14280.70640.50250.060*
H60.08990.60660.27510.064*
H70.24750.52800.23420.064*
H80.10390.43280.43930.059*
H90.08580.34300.31170.059*
H100.19310.21460.53520.010*0.19 (3)
H110.38860.17350.56120.010*0.19
H120.26520.10450.44360.010*0.19
H130.26260.22840.57470.045*0.81
H140.19470.13520.45120.045*0.81
H150.38950.12910.51410.045*0.81
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Br10.0526 (4)0.0413 (4)0.0344 (4)0.00196 (8)0.0233 (2)0.00341 (8)
Ni10.0274 (5)0.0264 (6)0.0278 (5)0.0011 (1)0.0102 (3)0.0003 (2)
N10.0376 (10)0.0302 (11)0.0311 (10)0.0052 (8)0.0106 (8)0.0036 (9)
N20.0363 (10)0.0317 (12)0.0413 (11)0.0013 (8)0.0110 (8)0.0087 (9)
C10.0375 (12)0.046 (2)0.062 (2)0.0069 (10)0.0004 (10)0.001 (1)
C20.049 (1)0.052 (2)0.053 (2)0.002 (2)0.0051 (11)0.006 (2)
C30.058 (2)0.032 (1)0.050 (1)0.0109 (12)0.0185 (11)0.0031 (13)
C40.053 (2)0.042 (2)0.061 (2)0.0128 (11)0.0276 (13)0.009 (1)
Geometric parameters (Å, º) top
Ni1—Br12.6712 (4)C1—H80.950
Ni1—Br1i2.6712 (4)C1—H90.950
Ni1—N12.119 (2)C2—H60.950
Ni1—N1i2.119 (2)C2—H70.950
Ni1—N22.127 (2)C3—H100.952
Ni1—N2i2.127 (2)C3—H110.948
N1—C11.477 (3)C3—H120.949
N1—C31.460 (4)C3—H130.951
N2—C21.482 (4)C3—H140.951
N2—C41.462 (4)C3—H150.947
C1—C21.495 (5)C4—H30.950
N1—H20.950C4—H40.950
N2—H10.950C4—H50.950
Br1···N2ii3.603 (2)Br1···C4ii3.708 (3)
Br1···C3iii3.665 (3)C3···C4iv3.776 (5)
Br1···N1iii3.705 (2)
Br1—Ni1—Br1i180.00N1—C1—H8109.31
Br1—Ni1—N190.72 (6)N1—C1—H9109.31
Br1—Ni1—N1i89.28 (6)C2—C1—H8109.32
Br1—Ni1—N294.65 (7)C2—C1—H9109.31
Br1—Ni1—N2i85.35 (7)H8—C1—H9109.46
Br1i—Ni1—N189.28 (6)N2—C2—H6109.41
Br1i—Ni1—N1i90.72 (6)N2—C2—H7109.41
Br1i—Ni1—N285.35 (7)C1—C2—H6109.41
Br1i—Ni1—N2i94.65 (7)C1—C2—H7109.42
N1—Ni1—N1i180.00H6—C2—H7109.46
N1—Ni1—N284.2 (1)N1—C3—H10109.3
N1—Ni1—N2i95.8 (1)N1—C3—H11109.6
N1i—Ni1—N295.8 (1)N1—C3—H12109.6
N1i—Ni1—N2i84.2 (1)N1—C3—H13109.3
N2—Ni1—N2i180.00N1—C3—H14109.4
Ni1—N1—C1105.1 (2)N1—C3—H15109.6
Ni1—N1—C3120.6 (2)H10—C3—H11109.4
C1—N1—C3110.1 (2)H10—C3—H12109.3
Ni1—N2—C2105.3 (2)H11—C3—H12109.7
Ni1—N2—C4118.9 (2)H13—C3—H14109.2
C2—N2—C4113.2 (2)H13—C3—H15109.6
N1—C1—C2110.1 (2)H14—C3—H15109.6
N2—C2—C1109.7 (3)N2—C4—H3109.48
Ni1—N1—H2106.76N2—C4—H4109.47
C1—N1—H2106.77N2—C4—H5109.47
C3—N1—H2106.76H3—C4—H4109.47
Ni1—N2—H1106.19H3—C4—H5109.48
C2—N2—H1106.19H4—C4—H5109.47
C4—N2—H1106.20
Br1—Ni1—N1—C179.4 (2)N1—Ni1—N2—C213.6 (2)
Br1—Ni1—N1—C345.6 (2)N1—Ni1—N2—C4114.5 (2)
Br1—Ni1—N1i—C1i100.6 (2)N1—Ni1—N2i—C2i166.4 (2)
Br1—Ni1—N1i—C3i134.4 (2)N1—Ni1—N2i—C4i65.5 (2)
Br1—Ni1—N2—C2103.9 (2)N1—C1—C2—N258.3 (4)
Br1—Ni1—N2—C424.3 (2)N2—Ni1—N1—C115.2 (2)
Br1—Ni1—N2i—C2i76.1 (2)N2—Ni1—N1—C3140.2 (2)
Br1—Ni1—N2i—C4i155.7 (2)N2—Ni1—N1i—C1i164.8 (2)
Ni1—N1—C1—C242.4 (3)N2—Ni1—N1i—C3i39.8 (2)
Ni1—N1i—C1i—C2i42.4 (3)C1—C2—N2—C490.8 (3)
Ni1—N2—C2—C140.7 (3)C2—C1—N1—C3173.7 (3)
Ni1—N2i—C2i—C1i40.7 (3)
Symmetry codes: (i) x+1, y+1, z+1; (ii) x, y+3/2, z+1/2; (iii) x, y+1/2, z+1/2; (iv) x, y1, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N2—H1···Br1v0.952.803.603 (2)143
N1—H2···Br1vi0.952.933.705 (2)139
Symmetry codes: (v) x, y+3/2, z1/2; (vi) x, y+1/2, z1/2.
 

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