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The title compound, [NiCl2(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 chloride 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/S1600536806033770/bv2026sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536806033770/bv2026Isup2.hkl
Contains datablock I

CCDC reference: 620707

Key indicators

  • Single-crystal X-ray study
  • T = 100 K
  • Mean [sigma](C-C) = 0.001 Å
  • R factor = 0.032
  • wR factor = 0.081
  • Data-to-parameter ratio = 33.9

checkCIF/PLATON results

No syntax errors found



Alert level A PLAT222_ALERT_3_A Large Non-Solvent H Ueq(max)/Ueq(min) ... 10.00 Ratio
Author Response: see _publ_section_exptl_refinement. One methyl group is disordered, so one set of H atoms has a small Ueq producing a small Ueq(min).

Alert level B PLAT110_ALERT_2_B ADDSYM Detects Potential Lattice Centering or Halving . ?
Alert level C PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Ni1 - N1 .. 9.09 su PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Ni1 - N2 .. 8.18 su PLAT245_ALERT_2_C U(iso) H3 Smaller than U(eq) C3 by ... 0.01 AngSq PLAT245_ALERT_2_C U(iso) H4 Smaller than U(eq) C3 by ... 0.01 AngSq PLAT245_ALERT_2_C U(iso) H5 Smaller than U(eq) C3 by ... 0.01 AngSq PLAT420_ALERT_2_C D-H Without Acceptor N1 - H1 ... ? PLAT480_ALERT_4_C Long H...A H-Bond Reported H1 .. CL1 .. 2.85 Ang.
1 ALERT level A = In general: serious problem 1 ALERT level B = Potentially serious problem 7 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 7 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 1 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check

Computing details top

Data collection: COLLECT (Nonius, 2000); cell refinement: SCALEPACK (Otwinowski & Minor, 1997); data reduction: SCALEPACK and DENZO (Otwinowski & Minor, 1997); program(s) used to solve structure: SIR92 (Altomare et al., 1993); program(s) used to refine structure: TEXSAN for Windows (Molecular Structure Corporation, 1999); molecular graphics: PROGRAM? (Reference?); software used to prepare material for publication: TEXSAN for Windows.

trans-Dichlorobis(N,N'-dimethylethane-1,2-diamine-κ2N,N')nickel(II) top
Crystal data top
[NiCl2(C4H12N2)2]F(000) = 324.00
Mr = 305.91Dx = 1.526 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.7107 Å
Hall symbol: -P 2ybcCell parameters from 2953 reflections
a = 7.8639 (2) Åθ = 2.5–35.0°
b = 8.5786 (2) ŵ = 1.84 mm1
c = 10.0186 (3) ÅT = 100 K
β = 99.9252 (10)°Fragment, blue
V = 665.75 (3) Å30.35 × 0.30 × 0.27 mm
Z = 2
Data collection top
Nonius KappaCCD (with an Oxford Cryosystem Cryostream coller)
diffractometer
2918 independent reflections
Radiation source: fine-focus sealed tube2435 reflections with I > 3σ(I)
Graphite monochromatorRint = 0.013
ω scans with κ offsetsθmax = 35.0°, θmin = 3.1°
Absorption correction: multi-scan
(SCALEPACK; Otwinowski & Minor, 1997)
h = 1212
Tmin = 0.552, Tmax = 0.609k = 1311
15248 measured reflectionsl = 1616
Refinement top
Refinement on F25 constraints
Least-squares matrix: fullH-atom parameters constrained
R[F2 > 2σ(F2)] = 0.032Weighting scheme based on measured s.u.'s w = 1/[σ2(Fo) + 0.0009|Fo|2]
wR(F2) = 0.081(Δ/σ)max = 0.001
S = 0.99Δρmax = 0.58 e Å3
2440 reflectionsΔρmin = 0.56 e Å3
72 parametersExtinction correction: Zachariasen (1967), equ(3) Acta Cryst.(1968) A24, p213.
0 restraintsExtinction coefficient: 0.0000028 (5)
Special details top

Experimental. Absorption spectrum (water) λmax (εM): 361.7 (12.8), 588.1 (7.2), 966.2 (7.1). 1H NMR (300 MHz, D2O): δ 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)
Ni10.50000.50000.50000.00892 (5)
Cl10.62467 (3)0.50959 (2)0.28817 (2)0.01420 (6)
N10.67963 (9)0.32511 (8)0.57977 (7)0.0119 (1)
N20.68319 (9)0.65571 (8)0.60917 (7)0.0125 (1)
C10.84251 (10)0.40946 (9)0.62702 (9)0.0154 (2)
C20.80566 (11)0.55670 (10)0.70081 (8)0.0166 (2)
C30.71104 (11)0.19213 (10)0.49432 (9)0.0164 (2)
C40.77160 (12)0.76410 (10)0.52974 (9)0.0172 (2)
H10.64220.28360.65770.014*
H20.62330.71750.66470.015*
H30.73080.10080.54840.002*0.086 (12)
H40.61350.17680.42530.002*0.086
H50.80970.21280.45400.002*0.086
H60.91860.34460.68680.018*
H70.89470.43620.55140.018*
H80.91020.61220.72880.020*
H90.75670.52980.77800.020*
H100.85140.70790.48690.021*
H110.68890.81360.46280.021*
H120.83160.84070.58830.021*
H130.73900.22950.41140.018*0.914
H140.61050.12920.47590.018*0.914
H150.80450.13170.54030.018*0.914
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ni10.01138 (10)0.00735 (9)0.00846 (10)0.00062 (4)0.00295 (7)0.00018 (4)
Cl10.01960 (13)0.01337 (11)0.01108 (12)0.00103 (6)0.00677 (9)0.00155 (5)
N10.0152 (3)0.0091 (3)0.0119 (3)0.0008 (2)0.0039 (2)0.0001 (2)
N20.0148 (3)0.0094 (3)0.0136 (3)0.0005 (2)0.0033 (2)0.0008 (2)
C10.0138 (4)0.0129 (3)0.0184 (4)0.0018 (3)0.0001 (3)0.0008 (3)
C20.0194 (4)0.0134 (3)0.0153 (4)0.0000 (3)0.0015 (3)0.0020 (3)
C30.0211 (4)0.0100 (3)0.0183 (4)0.0030 (3)0.0041 (3)0.0016 (3)
C40.0192 (4)0.0122 (3)0.0213 (4)0.0028 (3)0.0066 (3)0.0002 (3)
Geometric parameters (Å, º) top
Ni1—Cl12.4878 (2)C1—H60.950
Ni1—Cl1i2.4878 (2)C1—H70.950
Ni1—N12.1204 (7)C2—H80.950
Ni1—N1i2.1204 (7)C2—H90.950
Ni1—N22.1243 (7)C3—H30.950
Ni1—N2i2.1243 (7)C3—H40.949
N1—C11.476 (1)C3—H50.951
N1—C31.472 (1)C3—H130.951
N2—C21.479 (1)C3—H140.949
N2—C41.474 (1)C3—H150.951
C1—C21.517 (1)C4—H100.950
N1—H10.950C4—H110.950
N2—H20.950C4—H120.950
Cl1···N2ii3.4578 (7)Cl1···C4ii3.5831 (9)
Cl1···C3iii3.5793 (9)
Cl1—Ni1—Cl1i180.00N1—C1—H6109.43
Cl1—Ni1—N190.57 (2)N1—C1—H7109.43
Cl1—Ni1—N1i89.43 (2)C2—C1—H6109.43
Cl1—Ni1—N294.96 (2)C2—C1—H7109.43
Cl1—Ni1—N2i85.04 (2)H6—C1—H7109.46
Cl1i—Ni1—N189.43 (2)N2—C2—H8109.46
Cl1i—Ni1—N1i90.57 (2)N2—C2—H9109.46
Cl1i—Ni1—N285.04 (2)C1—C2—H8109.46
Cl1i—Ni1—N2i94.96 (2)C1—C2—H9109.46
N1—Ni1—N1i180.00H8—C2—H9109.46
N1—Ni1—N284.39 (3)N1—C3—H3109.58
N1—Ni1—N2i95.61 (3)N1—C3—H4109.60
N1i—Ni1—N295.61 (3)N1—C3—H5109.47
N1i—Ni1—N2i84.39 (3)N1—C3—H13109.51
N2—Ni1—N2i180.00N1—C3—H14109.63
Ni1—N1—C1105.01 (5)N1—C3—H15109.52
Ni1—N1—C3119.78 (5)H3—C3—H4109.48
C1—N1—C3110.06 (6)H3—C3—H5109.30
Ni1—N2—C2105.65 (5)H4—C3—H5109.39
Ni1—N2—C4117.38 (5)H13—C3—H14109.46
C2—N2—C4112.35 (7)H13—C3—H15109.29
N1—C1—C2109.66 (7)H14—C3—H15109.42
N2—C2—C1109.54 (7)N2—C4—H10109.47
Ni1—N1—H1107.12N2—C4—H11109.47
C1—N1—H1107.13N2—C4—H12109.47
C3—N1—H1107.12H10—C4—H11109.47
Ni1—N2—H2106.98H10—C4—H12109.47
C2—N2—H2106.97H11—C4—H12109.47
C4—N2—H2106.98
Ni1—N1—C1—C243.15 (7)N1—Ni1—N2—C212.87 (5)
Ni1—N1i—C1i—C2i43.15 (7)N1—Ni1—N2—C4113.28 (6)
Ni1—N2—C2—C139.99 (8)N1—Ni1—N2i—C2i167.13 (5)
Ni1—N2i—C2i—C1i39.99 (8)N1—Ni1—N2i—C4i66.73 (6)
Cl1—Ni1—N1—C178.48 (5)N1—C1—C2—N258.30 (9)
Cl1—Ni1—N1—C345.76 (6)N2—Ni1—N1—C116.45 (5)
Cl1—Ni1—N1i—C1i101.52 (5)N2—Ni1—N1—C3140.68 (6)
Cl1—Ni1—N1i—C3i134.24 (6)N2—Ni1—N1i—C1i163.55 (5)
Cl1—Ni1—N2—C2102.96 (5)N2—Ni1—N1i—C3i39.32 (6)
Cl1—Ni1—N2—C423.18 (6)C1—C2—N2—C489.18 (8)
Cl1—Ni1—N2i—C2i77.04 (5)C2—C1—N1—C3173.34 (7)
Cl1—Ni1—N2i—C4i156.82 (6)
Symmetry codes: (i) x+1, y+1, z+1; (ii) x, y+3/2, z1/2; (iii) x, y+1/2, z1/2.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N2—H2···Cl1iv0.952.653.4578 (7)144
N1—H1···Cl1v0.952.853.6196 (7)139
Symmetry codes: (iv) x, y+3/2, z+1/2; (v) x, y+1/2, z+1/2.
 

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