Buy article online - an online subscription or single-article purchase is required to access this article.
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
CCDC reference: 620707
Key indicators
- Single-crystal X-ray study
- T = 100 K
- Mean (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
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 = 305.91 | Dx = 1.526 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.7107 Å |
Hall symbol: -P 2ybc | Cell parameters from 2953 reflections |
a = 7.8639 (2) Å | θ = 2.5–35.0° |
b = 8.5786 (2) Å | µ = 1.84 mm−1 |
c = 10.0186 (3) Å | T = 100 K |
β = 99.9252 (10)° | Fragment, blue |
V = 665.75 (3) Å3 | 0.35 × 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 tube | 2435 reflections with I > 3σ(I) |
Graphite monochromator | Rint = 0.013 |
ω scans with κ offsets | θmax = 35.0°, θmin = 3.1° |
Absorption correction: multi-scan (SCALEPACK; Otwinowski & Minor, 1997) | h = −12→12 |
Tmin = 0.552, Tmax = 0.609 | k = −13→11 |
15248 measured reflections | l = −16→16 |
Refinement top
Refinement on F2 | 5 constraints |
Least-squares matrix: full | H-atom parameters constrained |
R[F2 > 2σ(F2)] = 0.032 | Weighting 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 = 0.99 | Δρmax = 0.58 e Å−3 |
2440 reflections | Δρmin = −0.56 e Å−3 |
72 parameters | Extinction correction: Zachariasen (1967), equ(3) Acta Cryst.(1968) A24, p213. |
0 restraints | Extinction 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 | x | y | z | Uiso*/Ueq | Occ. (<1) |
Ni1 | 0.5000 | 0.5000 | 0.5000 | 0.00892 (5) | |
Cl1 | 0.62467 (3) | 0.50959 (2) | 0.28817 (2) | 0.01420 (6) | |
N1 | 0.67963 (9) | 0.32511 (8) | 0.57977 (7) | 0.0119 (1) | |
N2 | 0.68319 (9) | 0.65571 (8) | 0.60917 (7) | 0.0125 (1) | |
C1 | 0.84251 (10) | 0.40946 (9) | 0.62702 (9) | 0.0154 (2) | |
C2 | 0.80566 (11) | 0.55670 (10) | 0.70081 (8) | 0.0166 (2) | |
C3 | 0.71104 (11) | 0.19213 (10) | 0.49432 (9) | 0.0164 (2) | |
C4 | 0.77160 (12) | 0.76410 (10) | 0.52974 (9) | 0.0172 (2) | |
H1 | 0.6422 | 0.2836 | 0.6577 | 0.014* | |
H2 | 0.6233 | 0.7175 | 0.6647 | 0.015* | |
H3 | 0.7308 | 0.1008 | 0.5484 | 0.002* | 0.086 (12) |
H4 | 0.6135 | 0.1768 | 0.4253 | 0.002* | 0.086 |
H5 | 0.8097 | 0.2128 | 0.4540 | 0.002* | 0.086 |
H6 | 0.9186 | 0.3446 | 0.6868 | 0.018* | |
H7 | 0.8947 | 0.4362 | 0.5514 | 0.018* | |
H8 | 0.9102 | 0.6122 | 0.7288 | 0.020* | |
H9 | 0.7567 | 0.5298 | 0.7780 | 0.020* | |
H10 | 0.8514 | 0.7079 | 0.4869 | 0.021* | |
H11 | 0.6889 | 0.8136 | 0.4628 | 0.021* | |
H12 | 0.8316 | 0.8407 | 0.5883 | 0.021* | |
H13 | 0.7390 | 0.2295 | 0.4114 | 0.018* | 0.914 |
H14 | 0.6105 | 0.1292 | 0.4759 | 0.018* | 0.914 |
H15 | 0.8045 | 0.1317 | 0.5403 | 0.018* | 0.914 |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Ni1 | 0.01138 (10) | 0.00735 (9) | 0.00846 (10) | 0.00062 (4) | 0.00295 (7) | 0.00018 (4) |
Cl1 | 0.01960 (13) | 0.01337 (11) | 0.01108 (12) | 0.00103 (6) | 0.00677 (9) | 0.00155 (5) |
N1 | 0.0152 (3) | 0.0091 (3) | 0.0119 (3) | 0.0008 (2) | 0.0039 (2) | 0.0001 (2) |
N2 | 0.0148 (3) | 0.0094 (3) | 0.0136 (3) | 0.0005 (2) | 0.0033 (2) | −0.0008 (2) |
C1 | 0.0138 (4) | 0.0129 (3) | 0.0184 (4) | 0.0018 (3) | −0.0001 (3) | 0.0008 (3) |
C2 | 0.0194 (4) | 0.0134 (3) | 0.0153 (4) | 0.0000 (3) | −0.0015 (3) | −0.0020 (3) |
C3 | 0.0211 (4) | 0.0100 (3) | 0.0183 (4) | 0.0030 (3) | 0.0041 (3) | −0.0016 (3) |
C4 | 0.0192 (4) | 0.0122 (3) | 0.0213 (4) | −0.0028 (3) | 0.0066 (3) | −0.0002 (3) |
Geometric parameters (Å, º) top
Ni1—Cl1 | 2.4878 (2) | C1—H6 | 0.950 |
Ni1—Cl1i | 2.4878 (2) | C1—H7 | 0.950 |
Ni1—N1 | 2.1204 (7) | C2—H8 | 0.950 |
Ni1—N1i | 2.1204 (7) | C2—H9 | 0.950 |
Ni1—N2 | 2.1243 (7) | C3—H3 | 0.950 |
Ni1—N2i | 2.1243 (7) | C3—H4 | 0.949 |
N1—C1 | 1.476 (1) | C3—H5 | 0.951 |
N1—C3 | 1.472 (1) | C3—H13 | 0.951 |
N2—C2 | 1.479 (1) | C3—H14 | 0.949 |
N2—C4 | 1.474 (1) | C3—H15 | 0.951 |
C1—C2 | 1.517 (1) | C4—H10 | 0.950 |
N1—H1 | 0.950 | C4—H11 | 0.950 |
N2—H2 | 0.950 | C4—H12 | 0.950 |
| | | |
Cl1···N2ii | 3.4578 (7) | Cl1···C4ii | 3.5831 (9) |
Cl1···C3iii | 3.5793 (9) | | |
| | | |
Cl1—Ni1—Cl1i | 180.00 | N1—C1—H6 | 109.43 |
Cl1—Ni1—N1 | 90.57 (2) | N1—C1—H7 | 109.43 |
Cl1—Ni1—N1i | 89.43 (2) | C2—C1—H6 | 109.43 |
Cl1—Ni1—N2 | 94.96 (2) | C2—C1—H7 | 109.43 |
Cl1—Ni1—N2i | 85.04 (2) | H6—C1—H7 | 109.46 |
Cl1i—Ni1—N1 | 89.43 (2) | N2—C2—H8 | 109.46 |
Cl1i—Ni1—N1i | 90.57 (2) | N2—C2—H9 | 109.46 |
Cl1i—Ni1—N2 | 85.04 (2) | C1—C2—H8 | 109.46 |
Cl1i—Ni1—N2i | 94.96 (2) | C1—C2—H9 | 109.46 |
N1—Ni1—N1i | 180.00 | H8—C2—H9 | 109.46 |
N1—Ni1—N2 | 84.39 (3) | N1—C3—H3 | 109.58 |
N1—Ni1—N2i | 95.61 (3) | N1—C3—H4 | 109.60 |
N1i—Ni1—N2 | 95.61 (3) | N1—C3—H5 | 109.47 |
N1i—Ni1—N2i | 84.39 (3) | N1—C3—H13 | 109.51 |
N2—Ni1—N2i | 180.00 | N1—C3—H14 | 109.63 |
Ni1—N1—C1 | 105.01 (5) | N1—C3—H15 | 109.52 |
Ni1—N1—C3 | 119.78 (5) | H3—C3—H4 | 109.48 |
C1—N1—C3 | 110.06 (6) | H3—C3—H5 | 109.30 |
Ni1—N2—C2 | 105.65 (5) | H4—C3—H5 | 109.39 |
Ni1—N2—C4 | 117.38 (5) | H13—C3—H14 | 109.46 |
C2—N2—C4 | 112.35 (7) | H13—C3—H15 | 109.29 |
N1—C1—C2 | 109.66 (7) | H14—C3—H15 | 109.42 |
N2—C2—C1 | 109.54 (7) | N2—C4—H10 | 109.47 |
Ni1—N1—H1 | 107.12 | N2—C4—H11 | 109.47 |
C1—N1—H1 | 107.13 | N2—C4—H12 | 109.47 |
C3—N1—H1 | 107.12 | H10—C4—H11 | 109.47 |
Ni1—N2—H2 | 106.98 | H10—C4—H12 | 109.47 |
C2—N2—H2 | 106.97 | H11—C4—H12 | 109.47 |
C4—N2—H2 | 106.98 | | |
| | | |
Ni1—N1—C1—C2 | 43.15 (7) | N1—Ni1—N2—C2 | −12.87 (5) |
Ni1—N1i—C1i—C2i | −43.15 (7) | N1—Ni1—N2—C4 | 113.28 (6) |
Ni1—N2—C2—C1 | 39.99 (8) | N1—Ni1—N2i—C2i | −167.13 (5) |
Ni1—N2i—C2i—C1i | −39.99 (8) | N1—Ni1—N2i—C4i | 66.73 (6) |
Cl1—Ni1—N1—C1 | 78.48 (5) | N1—C1—C2—N2 | −58.30 (9) |
Cl1—Ni1—N1—C3 | −45.76 (6) | N2—Ni1—N1—C1 | −16.45 (5) |
Cl1—Ni1—N1i—C1i | 101.52 (5) | N2—Ni1—N1—C3 | −140.68 (6) |
Cl1—Ni1—N1i—C3i | −134.24 (6) | N2—Ni1—N1i—C1i | −163.55 (5) |
Cl1—Ni1—N2—C2 | −102.96 (5) | N2—Ni1—N1i—C3i | −39.32 (6) |
Cl1—Ni1—N2—C4 | 23.18 (6) | C1—C2—N2—C4 | −89.18 (8) |
Cl1—Ni1—N2i—C2i | −77.04 (5) | C2—C1—N1—C3 | 173.34 (7) |
Cl1—Ni1—N2i—C4i | 156.82 (6) | | |
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. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
N2—H2···Cl1iv | 0.95 | 2.65 | 3.4578 (7) | 144 |
N1—H1···Cl1v | 0.95 | 2.85 | 3.6196 (7) | 139 |
Symmetry codes: (iv) x, −y+3/2, z+1/2; (v) x, −y+1/2, z+1/2. |
Subscribe to Acta Crystallographica Section E: Crystallographic Communications
The full text of this article is available to subscribers to the journal.
If you have already registered and are using a computer listed in your registration details, please email
support@iucr.org for assistance.