


Supporting information
![]() | Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807066913/hy2111sup1.cif |
![]() | Structure factor file (CIF format) https://doi.org/10.1107/S1600536807066913/hy2111Isup2.hkl |
CCDC reference: 674257
Key indicators
- Single-crystal X-ray study
- T = 220 K
- Mean
(C-C) = 0.015 Å
- Disorder in main residue
- R factor = 0.034
- wR factor = 0.084
- Data-to-parameter ratio = 13.7
checkCIF/PLATON results
No syntax errors found
Alert level B PLAT230_ALERT_2_B Hirshfeld Test Diff for N21 - C21 .. 7.82 su PLAT241_ALERT_2_B Check High Ueq as Compared to Neighbors for C21 PLAT301_ALERT_3_B Main Residue Disorder ......................... 36.00 Perc.
Alert level C PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for C41 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for N21 PLAT244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for Pt PLAT342_ALERT_3_C Low Bond Precision on C-C Bonds (x 1000) Ang ... 16
0 ALERT level A = In general: serious problem 3 ALERT level B = Potentially serious problem 5 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 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 1 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check
The title compound were prepared by a chance during our attempts to prepare chain-like [Ni(pn)2][Pt(CN)4] compound suitable for magnetic studies. A mixture of a 10 ml aqueous solution of NiSO4.6H2O (0.132 g, 0.5 mmol) and pn (0.086 ml, 1.0 mmol) was stirred for 30 min and a 10 ml aqueous solution of K2[Pt(CN)4].3H2O (0.216 g, 0.5 mmol) was added. The pink precipitate thus formed was dissolved by addition of a concentrated solution of ammonia (20 ml). After few days, pink crystals of the title compound were filtered off and dried in air.
H atoms were positioned geometrically and refined as riding atoms, with N—H = 0.90 Å, C—H = 0.97Å (CH2), 0.98Å (CH) and Uiso(H) = 1.2Ueq(C,N) and with C—H = 0.96Å (CH3) and Uiso(H) = 1.5Ueq(C). The highest residual electron density and the deepest hole were found 1.01 and 0.88 Å from the Pt atom, respectively.
The title compound, [Ni(pn)3][Pt(CN)4] (pn = 1,2-diaminopropane) has been prepared by a chance within our studies on the role of hydrogen bonds as possible exchange paths for magnetic interactions in low-dimensional compounds. The compound consists of discrete [Ni(pn)3]2+ cations and [Pt(CN)4]2- anions (Fig. 1). Selected bond lengths and angles are given in Table 1. The NiII atom is coordinated by six N atoms of three racemic pn ligands, which are disordered over two sets of positions, with site occupancies of 0.50 (except methylene and methine C atoms), thus forming Δ(δδδ) and Δ(λλλ) configurations. Moreover, a mirror plane passes through the tetracyanoplatinate anion (N1, C1, Pt, C2 and N2 atoms) and the [Ni(pn)3]2+ cation (Ni, C31 and C41 atoms). The coordination geometry around the NiII atom can be described as octahedral. The two N atoms occupying axial positions form an angle of 170.6 (4)° and the Ni—N bond distances range from 2.118 (9)–2.142 (10)Å [mean bond length is 2.131 (10) Å], in good agreement with the values reported of other [Ni(pn)3]2+ complexes (Behrens et al., 2003; Kuchár & Černák, 2008; Saha et al., 2005). Octahedral coordination geometry around the Ni atom was observed also in other compounds with [Ni(pn)3]2+ cation (Nasanen et al., 1964; Lin et al., 2005). The square-planar geometry of [Pt(CN)4]2- is in good agreement with those of the previous studies with average Pt—C bond lengths of 1.988 (10) Å. The structure is stabilized also by the N—H···N hydrogen bonds between the cations and anions (Table 2).
For related literature on compounds with [Ni(1,2-diaminopropane)3]2+ cations, see: Behrens et al. (2003) for Sn2S64-; Kuchár & Černák (2008) for [Ni(CN)4]2-; Lin et al. (2005) for [H3Ge14NiO27]4-; Nasanen et al. (1964) for ClO4-; Saha et al. (2005) for [Fe(CN)5NO]2-.
Data collection: IPDS EXPOSE (Stoe & Cie, 1999); cell refinement: IPDS CELL (Stoe & Cie, 1999); data reduction: IPDS INTEGRATE (Stoe & Cie, 1999); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: DIAMOND (Brandenburg, 2001); software used to prepare material for publication: SHELXL97 (Sheldrick, 1997).
[Ni(C3H10N2)3][Pt(CN)4] | F(000) = 1136 |
Mr = 580.27 | Dx = 1.762 Mg m−3 |
Orthorhombic, Pnma | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ac 2n | Cell parameters from 8000 reflections |
a = 9.8206 (18) Å | θ = 2.4–25.9° |
b = 13.694 (2) Å | µ = 7.27 mm−1 |
c = 16.261 (3) Å | T = 220 K |
V = 2186.8 (7) Å3 | Needle, pink |
Z = 4 | 0.38 × 0.11 × 0.06 mm |
Stoe IPDS diffractometer | 2197 independent reflections |
Radiation source: fine-focus sealed tube | 1807 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.088 |
φ scans | θmax = 25.9°, θmin = 2.4° |
Absorption correction: numerical (IPDS FACE; Stoe & Cie, 1999) | h = −12→12 |
Tmin = 0.104, Tmax = 0.446 | k = −16→16 |
15408 measured reflections | l = −19→19 |
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.034 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.085 | H-atom parameters constrained |
S = 1.04 | w = 1/[σ2(Fo2) + (0.0507P)2] where P = (Fo2 + 2Fc2)/3 |
2197 reflections | (Δ/σ)max < 0.001 |
160 parameters | Δρmax = 1.23 e Å−3 |
0 restraints | Δρmin = −1.92 e Å−3 |
[Ni(C3H10N2)3][Pt(CN)4] | V = 2186.8 (7) Å3 |
Mr = 580.27 | Z = 4 |
Orthorhombic, Pnma | Mo Kα radiation |
a = 9.8206 (18) Å | µ = 7.27 mm−1 |
b = 13.694 (2) Å | T = 220 K |
c = 16.261 (3) Å | 0.38 × 0.11 × 0.06 mm |
Stoe IPDS diffractometer | 2197 independent reflections |
Absorption correction: numerical (IPDS FACE; Stoe & Cie, 1999) | 1807 reflections with I > 2σ(I) |
Tmin = 0.104, Tmax = 0.446 | Rint = 0.088 |
15408 measured reflections |
R[F2 > 2σ(F2)] = 0.034 | 0 restraints |
wR(F2) = 0.085 | H-atom parameters constrained |
S = 1.04 | Δρmax = 1.23 e Å−3 |
2197 reflections | Δρmin = −1.92 e Å−3 |
160 parameters |
x | y | z | Uiso*/Ueq | Occ. (<1) | |
Pt | 0.20444 (3) | 0.2500 | 0.07418 (2) | 0.04021 (13) | |
Ni | 0.73154 (10) | 0.2500 | 0.02973 (6) | 0.0368 (2) | |
C1 | 0.1023 (9) | 0.2500 | 0.1776 (5) | 0.0475 (19) | |
N1 | 0.0397 (9) | 0.2500 | 0.2376 (5) | 0.072 (2) | |
C2 | 0.3067 (9) | 0.2500 | −0.0318 (7) | 0.058 (2) | |
N2 | 0.3700 (10) | 0.2500 | −0.0916 (6) | 0.079 (3) | |
C3 | 0.2044 (8) | 0.1040 (6) | 0.0754 (5) | 0.069 (2) | |
N3 | 0.2032 (10) | 0.0220 (4) | 0.0777 (5) | 0.106 (3) | |
C21 | 0.6124 (10) | 0.4305 (6) | 0.0987 (7) | 0.104 (3) | |
H21A | 0.5531 | 0.4642 | 0.1370 | 0.124* | 0.50 |
H21B | 0.6074 | 0.4631 | 0.0458 | 0.124* | 0.50 |
H21C | 0.5802 | 0.4971 | 0.0931 | 0.124* | 0.50 |
H21D | 0.5536 | 0.3967 | 0.1372 | 0.124* | 0.50 |
N10 | 0.8434 (11) | 0.3735 (7) | 0.0711 (6) | 0.048 (2) | 0.50 |
H10A | 0.9198 | 0.3542 | 0.0970 | 0.058* | 0.50 |
H10B | 0.8672 | 0.4112 | 0.0281 | 0.058* | 0.50 |
N20 | 0.5722 (11) | 0.3283 (7) | 0.0909 (6) | 0.051 (2) | 0.50 |
H20A | 0.4945 | 0.3238 | 0.0617 | 0.062* | 0.50 |
H20B | 0.5575 | 0.3024 | 0.1410 | 0.062* | 0.50 |
C11 | 0.7537 (11) | 0.4303 (6) | 0.1294 (6) | 0.085 (3) | |
H11A | 0.7449 | 0.3821 | 0.1737 | 0.101* | 0.50 |
H11B | 0.8156 | 0.4621 | 0.0905 | 0.101* | 0.50 |
N11 | 0.7811 (10) | 0.3348 (8) | 0.1363 (6) | 0.051 (3) | 0.50 |
H11C | 0.7346 | 0.3108 | 0.1795 | 0.061* | 0.50 |
H11D | 0.8704 | 0.3275 | 0.1471 | 0.061* | 0.50 |
N21 | 0.6087 (10) | 0.3743 (6) | 0.0070 (6) | 0.048 (2) | 0.50 |
H21E | 0.6445 | 0.4121 | −0.0328 | 0.057* | 0.50 |
H21F | 0.5234 | 0.3572 | −0.0071 | 0.057* | 0.50 |
C31 | 0.9053 (10) | 0.2500 | −0.1186 (6) | 0.067 (3) | |
H31 | 0.9357 | 0.3170 | −0.1082 | 0.081* | 0.50 |
C41 | 0.7596 (13) | 0.2500 | −0.1515 (6) | 0.087 (4) | |
H41A | 0.7236 | 0.1841 | −0.1547 | 0.104* | 0.50 |
H41B | 0.7551 | 0.2798 | −0.2056 | 0.104* | 0.50 |
N30 | 0.8963 (10) | 0.1956 (7) | −0.0412 (6) | 0.047 (2) | 0.50 |
H30A | 0.9746 | 0.2020 | −0.0128 | 0.056* | 0.50 |
H30B | 0.8835 | 0.1317 | −0.0517 | 0.056* | 0.50 |
N40 | 0.6798 (11) | 0.3121 (7) | −0.0867 (6) | 0.047 (2) | 0.50 |
H40A | 0.5895 | 0.3084 | −0.0956 | 0.057* | 0.50 |
H40B | 0.7054 | 0.3752 | −0.0890 | 0.057* | 0.50 |
C32 | 0.9945 (15) | 0.2029 (13) | −0.1810 (9) | 0.089 (5) | 0.50 |
H32A | 1.0867 | 0.2023 | −0.1615 | 0.134* | 0.50 |
H32B | 0.9898 | 0.2389 | −0.2316 | 0.134* | 0.50 |
H32C | 0.9644 | 0.1371 | −0.1903 | 0.134* | 0.50 |
C12 | 0.808 (3) | 0.5133 (17) | 0.1769 (16) | 0.101 (7) | 0.50 |
H12A | 0.9003 | 0.5003 | 0.1922 | 0.151* | 0.50 |
H12B | 0.7537 | 0.5224 | 0.2255 | 0.151* | 0.50 |
H12C | 0.8041 | 0.5714 | 0.1438 | 0.151* | 0.50 |
C13 | 0.721 (3) | 0.4965 (18) | 0.2020 (17) | 0.101 (7) | 0.50 |
H13A | 0.8029 | 0.5079 | 0.2332 | 0.151* | 0.50 |
H13B | 0.6546 | 0.4658 | 0.2364 | 0.151* | 0.50 |
H13C | 0.6867 | 0.5576 | 0.1821 | 0.151* | 0.50 |
U11 | U22 | U33 | U12 | U13 | U23 | |
Pt | 0.0384 (2) | 0.02827 (17) | 0.0540 (2) | 0.000 | −0.00989 (13) | 0.000 |
Ni | 0.0390 (5) | 0.0239 (5) | 0.0476 (5) | 0.000 | −0.0062 (4) | 0.000 |
C1 | 0.048 (5) | 0.040 (4) | 0.055 (5) | 0.000 | −0.006 (4) | 0.000 |
N1 | 0.073 (6) | 0.080 (7) | 0.064 (5) | 0.000 | −0.008 (5) | 0.000 |
C2 | 0.041 (5) | 0.064 (6) | 0.068 (6) | 0.000 | −0.013 (5) | 0.000 |
N2 | 0.048 (5) | 0.117 (9) | 0.072 (6) | 0.000 | 0.005 (4) | 0.000 |
C3 | 0.076 (6) | 0.057 (5) | 0.074 (4) | 0.005 (4) | 0.001 (4) | −0.007 (4) |
N3 | 0.177 (11) | 0.016 (3) | 0.124 (6) | 0.004 (4) | 0.013 (5) | −0.014 (3) |
C21 | 0.080 (6) | 0.044 (4) | 0.187 (10) | 0.005 (4) | 0.037 (7) | −0.042 (5) |
N10 | 0.044 (6) | 0.033 (5) | 0.066 (6) | −0.005 (4) | −0.014 (5) | −0.007 (5) |
N20 | 0.050 (6) | 0.046 (5) | 0.057 (6) | 0.007 (5) | −0.007 (5) | −0.005 (4) |
C11 | 0.104 (6) | 0.053 (5) | 0.097 (6) | −0.021 (5) | 0.015 (5) | −0.033 (4) |
N11 | 0.053 (7) | 0.045 (6) | 0.053 (5) | 0.000 (5) | −0.008 (5) | −0.003 (5) |
N21 | 0.047 (5) | 0.026 (4) | 0.070 (6) | −0.002 (4) | −0.015 (5) | −0.001 (4) |
C31 | 0.055 (6) | 0.085 (8) | 0.063 (6) | 0.000 | 0.007 (5) | 0.000 |
C41 | 0.065 (6) | 0.153 (13) | 0.043 (5) | 0.000 | 0.006 (5) | 0.000 |
N30 | 0.047 (6) | 0.035 (5) | 0.058 (5) | −0.002 (4) | −0.011 (4) | 0.005 (4) |
N40 | 0.046 (5) | 0.036 (5) | 0.059 (6) | −0.001 (4) | −0.013 (4) | 0.007 (4) |
C32 | 0.054 (8) | 0.124 (15) | 0.091 (10) | 0.021 (9) | 0.018 (8) | −0.005 (9) |
C12 | 0.14 (2) | 0.057 (9) | 0.110 (14) | 0.000 (12) | −0.024 (13) | −0.020 (9) |
C13 | 0.14 (2) | 0.057 (9) | 0.110 (14) | 0.000 (12) | −0.024 (13) | −0.020 (9) |
Pt—C1 | 1.958 (10) | N20—H20B | 0.9000 |
Pt—C2 | 1.995 (11) | C11—N11 | 1.340 (13) |
Pt—C3i | 1.999 (9) | C11—C13 | 1.52 (3) |
Pt—C3 | 1.999 (9) | C11—C12 | 1.47 (2) |
Ni—N21i | 2.118 (9) | C11—H11A | 0.9800 |
Ni—N21 | 2.118 (9) | C11—H11B | 0.9800 |
Ni—N10 | 2.127 (9) | N11—H11C | 0.9000 |
Ni—N10i | 2.127 (9) | N11—H11D | 0.9000 |
Ni—N30i | 2.122 (10) | N21—H21E | 0.9000 |
Ni—N30 | 2.122 (10) | N21—H21F | 0.9000 |
Ni—N40i | 2.137 (9) | C31—N30 | 1.466 (12) |
Ni—N40 | 2.137 (9) | C31—C32 | 1.487 (16) |
Ni—N11 | 2.142 (10) | C31—C41 | 1.528 (16) |
Ni—N11i | 2.142 (10) | C31—H31 | 0.9800 |
Ni—N20 | 2.142 (10) | C41—N40 | 1.565 (13) |
Ni—N20i | 2.142 (10) | C41—H41A | 0.9700 |
C1—N1 | 1.154 (11) | C41—H41B | 0.9700 |
C2—N2 | 1.154 (13) | N30—H30A | 0.9000 |
C3—N3 | 1.124 (11) | N30—H30B | 0.9000 |
C21—N20 | 1.460 (13) | N40—H40A | 0.9000 |
C21—C11 | 1.474 (14) | N40—H40B | 0.9000 |
C21—N21 | 1.679 (13) | C32—H32A | 0.9600 |
C21—H21A | 0.9700 | C32—H32B | 0.9600 |
C21—H21B | 0.9700 | C32—H32C | 0.9600 |
C21—H21C | 0.9700 | C12—H12A | 0.9600 |
C21—H21D | 0.9700 | C12—H12B | 0.9600 |
N10—C11 | 1.509 (14) | C12—H12C | 0.9600 |
N10—H10A | 0.9000 | C13—H13A | 0.9600 |
N10—H10B | 0.9000 | C13—H13B | 0.9600 |
N20—H20A | 0.9000 | C13—H13C | 0.9600 |
C1—Pt—C2 | 179.4 (3) | N11—C11—C13 | 124.0 (13) |
C1—Pt—C3i | 89.5 (2) | C21—C11—C13 | 93.8 (12) |
C2—Pt—C3i | 90.5 (2) | C21—C11—C12 | 120.9 (13) |
C1—Pt—C3 | 89.5 (2) | N10—C11—C12 | 121.1 (13) |
C2—Pt—C3 | 90.5 (2) | C21—C11—H11A | 99.6 |
C3i—Pt—C3 | 178.8 (4) | N10—C11—H11A | 99.6 |
N21i—Ni—N10 | 171.3 (4) | C12—C11—H11A | 99.6 |
N21—Ni—N10i | 171.3 (4) | N11—C11—H11B | 111.4 |
N21—Ni—N30i | 93.3 (4) | C21—C11—H11B | 111.4 |
N10i—Ni—N30i | 93.3 (4) | C13—C11—H11B | 111.4 |
N21i—Ni—N30 | 93.3 (4) | C11—N11—Ni | 114.6 (7) |
N10—Ni—N30 | 93.3 (4) | C11—N11—H11C | 108.6 |
N21—Ni—N40i | 91.7 (4) | Ni—N11—H11C | 108.6 |
N10i—Ni—N40i | 95.0 (4) | C11—N11—H11D | 108.6 |
N30i—Ni—N40i | 80.8 (4) | Ni—N11—H11D | 108.6 |
N21i—Ni—N40 | 91.7 (4) | H11C—N11—H11D | 107.6 |
N10—Ni—N40 | 95.0 (4) | C21—N21—Ni | 101.6 (6) |
N30—Ni—N40 | 80.8 (4) | C21—N21—H21E | 111.5 |
N21—Ni—N11 | 80.5 (4) | Ni—N21—H21E | 111.5 |
N10i—Ni—N11 | 93.3 (4) | C21—N21—H21F | 111.5 |
N30i—Ni—N11 | 94.4 (4) | Ni—N21—H21F | 111.5 |
N40i—Ni—N11 | 170.6 (4) | H21E—N21—H21F | 109.3 |
N21i—Ni—N11i | 80.5 (4) | N30—C31—C32 | 113.6 (8) |
N10—Ni—N11i | 93.3 (4) | N30—C31—C41 | 104.1 (7) |
N30—Ni—N11i | 94.4 (4) | C32—C31—C41 | 108.2 (9) |
N40—Ni—N11i | 170.6 (4) | N30—C31—H31 | 110.2 |
N21i—Ni—N20 | 93.8 (4) | C32—C31—H31 | 110.2 |
N10—Ni—N20 | 80.4 (4) | C41—C31—H31 | 110.2 |
N30—Ni—N20 | 170.1 (4) | C31—C41—N40 | 103.5 (7) |
N40—Ni—N20 | 92.2 (4) | C31—C41—H41A | 111.1 |
N11i—Ni—N20 | 93.5 (4) | N40—C41—H41A | 111.1 |
N21—Ni—N20i | 93.8 (4) | C31—C41—H41B | 111.1 |
N10i—Ni—N20i | 80.4 (4) | N40—C41—H41B | 111.1 |
N30i—Ni—N20i | 170.1 (4) | H41A—C41—H41B | 109.0 |
N40i—Ni—N20i | 92.2 (4) | C31—N30—Ni | 109.5 (6) |
N11—Ni—N20i | 93.5 (4) | C31—N30—H30A | 109.8 |
N1—C1—Pt | 178.6 (8) | Ni—N30—H30A | 109.8 |
N2—C2—Pt | 177.6 (8) | C31—N30—H30B | 109.8 |
N3—C3—Pt | 178.5 (8) | Ni—N30—H30B | 109.8 |
N20—C21—C11 | 106.4 (8) | H30A—N30—H30B | 108.2 |
C11—C21—N21 | 108.7 (7) | C41—N40—Ni | 105.2 (6) |
N20—C21—H21A | 110.4 | C41—N40—H40A | 110.7 |
C11—C21—H21A | 110.4 | Ni—N40—H40A | 110.7 |
N20—C21—H21B | 110.4 | C41—N40—H40B | 110.7 |
C11—C21—H21B | 110.4 | Ni—N40—H40B | 110.7 |
H21A—C21—H21B | 108.6 | H40A—N40—H40B | 108.8 |
C11—C21—H21C | 110.0 | C31—C32—H32A | 109.5 |
N21—C21—H21C | 110.0 | C31—C32—H32B | 109.5 |
C11—C21—H21D | 110.0 | H32A—C32—H32B | 109.5 |
N21—C21—H21D | 110.0 | C31—C32—H32C | 109.5 |
H21C—C21—H21D | 108.3 | H32A—C32—H32C | 109.5 |
C11—N10—Ni | 107.8 (7) | H32B—C32—H32C | 109.5 |
C11—N10—H10A | 110.1 | C11—C12—H12A | 109.5 |
Ni—N10—H10A | 110.1 | C11—C12—H12B | 109.5 |
C11—N10—H10B | 110.1 | H12A—C12—H12B | 109.5 |
Ni—N10—H10B | 110.1 | C11—C12—H12C | 109.5 |
H10A—N10—H10B | 108.5 | H12A—C12—H12C | 109.5 |
C21—N20—Ni | 108.8 (7) | H12B—C12—H12C | 109.5 |
C21—N20—H20A | 109.9 | C11—C13—H13A | 109.5 |
Ni—N20—H20A | 109.9 | C11—C13—H13B | 109.5 |
C21—N20—H20B | 109.9 | H13A—C13—H13B | 109.5 |
Ni—N20—H20B | 109.9 | C11—C13—H13C | 109.5 |
H20A—N20—H20B | 108.3 | H13A—C13—H13C | 109.5 |
N11—C11—C21 | 102.7 (8) | H13B—C13—H13C | 109.5 |
C21—C11—N10 | 109.7 (7) |
Symmetry code: (i) x, −y+1/2, z. |
D—H···A | D—H | H···A | D···A | D—H···A |
N21—H21F···N2 | 0.90 | 2.51 | 3.311 (12) | 148 |
N40—H40A···N2 | 0.90 | 2.30 | 3.160 (14) | 160 |
N10—H10B···N3ii | 0.90 | 2.40 | 3.193 (13) | 148 |
N21—H21E···N3ii | 0.90 | 2.24 | 3.066 (13) | 152 |
N40—H40B···N3ii | 0.90 | 2.21 | 3.098 (12) | 169 |
N11—H11C···N1iii | 0.90 | 2.48 | 3.342 (13) | 159 |
N20—H20B···N1iii | 0.90 | 2.11 | 3.005 (12) | 174 |
N11—H11D···N1iv | 0.90 | 2.46 | 3.242 (13) | 145 |
N30—H30B···N3v | 0.90 | 2.31 | 3.191 (11) | 166 |
Symmetry codes: (ii) −x+1, y+1/2, −z; (iii) x+1/2, −y+1/2, −z+1/2; (iv) x+1, y, z; (v) −x+1, −y, −z. |
Experimental details
Crystal data | |
Chemical formula | [Ni(C3H10N2)3][Pt(CN)4] |
Mr | 580.27 |
Crystal system, space group | Orthorhombic, Pnma |
Temperature (K) | 220 |
a, b, c (Å) | 9.8206 (18), 13.694 (2), 16.261 (3) |
V (Å3) | 2186.8 (7) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 7.27 |
Crystal size (mm) | 0.38 × 0.11 × 0.06 |
Data collection | |
Diffractometer | Stoe IPDS |
Absorption correction | Numerical (IPDS FACE; Stoe & Cie, 1999) |
Tmin, Tmax | 0.104, 0.446 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 15408, 2197, 1807 |
Rint | 0.088 |
(sin θ/λ)max (Å−1) | 0.615 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.034, 0.085, 1.04 |
No. of reflections | 2197 |
No. of parameters | 160 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 1.23, −1.92 |
Computer programs: IPDS EXPOSE (Stoe & Cie, 1999), IPDS CELL (Stoe & Cie, 1999), IPDS INTEGRATE (Stoe & Cie, 1999), SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), DIAMOND (Brandenburg, 2001).
Pt—C1 | 1.958 (10) | Ni—N30 | 2.122 (10) |
Pt—C2 | 1.995 (11) | Ni—N40 | 2.137 (9) |
Pt—C3 | 1.999 (9) | Ni—N11i | 2.142 (10) |
Ni—N21i | 2.118 (9) | Ni—N20 | 2.142 (10) |
Ni—N10 | 2.127 (9) | ||
C1—Pt—C2 | 179.4 (3) | N21i—Ni—N11i | 80.5 (4) |
C1—Pt—C3 | 89.5 (2) | N10—Ni—N11i | 93.3 (4) |
C2—Pt—C3 | 90.5 (2) | N30—Ni—N11i | 94.4 (4) |
C3i—Pt—C3 | 178.8 (4) | N40—Ni—N11i | 170.6 (4) |
N21i—Ni—N10 | 171.3 (4) | N21i—Ni—N20 | 93.8 (4) |
N21i—Ni—N30 | 93.3 (4) | N10—Ni—N20 | 80.4 (4) |
N10—Ni—N30 | 93.3 (4) | N30—Ni—N20 | 170.1 (4) |
N21i—Ni—N40 | 91.7 (4) | N40—Ni—N20 | 92.2 (4) |
N10—Ni—N40 | 95.0 (4) | N11i—Ni—N20 | 93.5 (4) |
N30—Ni—N40 | 80.8 (4) |
Symmetry code: (i) x, −y+1/2, z. |
D—H···A | D—H | H···A | D···A | D—H···A |
N21—H21F···N2 | 0.90 | 2.51 | 3.311 (12) | 148.2 |
N40—H40A···N2 | 0.90 | 2.30 | 3.160 (14) | 159.9 |
N10—H10B···N3ii | 0.90 | 2.40 | 3.193 (13) | 147.8 |
N21—H21E···N3ii | 0.90 | 2.24 | 3.066 (13) | 151.7 |
N40—H40B···N3ii | 0.90 | 2.21 | 3.098 (12) | 169.3 |
N11—H11C···N1iii | 0.90 | 2.48 | 3.342 (13) | 159.4 |
N20—H20B···N1iii | 0.90 | 2.11 | 3.005 (12) | 174.4 |
N11—H11D···N1iv | 0.90 | 2.46 | 3.242 (13) | 145.3 |
N30—H30B···N3v | 0.90 | 2.31 | 3.191 (11) | 166.4 |
Symmetry codes: (ii) −x+1, y+1/2, −z; (iii) x+1/2, −y+1/2, −z+1/2; (iv) x+1, y, z; (v) −x+1, −y, −z. |
The title compound, [Ni(pn)3][Pt(CN)4] (pn = 1,2-diaminopropane) has been prepared by a chance within our studies on the role of hydrogen bonds as possible exchange paths for magnetic interactions in low-dimensional compounds. The compound consists of discrete [Ni(pn)3]2+ cations and [Pt(CN)4]2- anions (Fig. 1). Selected bond lengths and angles are given in Table 1. The NiII atom is coordinated by six N atoms of three racemic pn ligands, which are disordered over two sets of positions, with site occupancies of 0.50 (except methylene and methine C atoms), thus forming Δ(δδδ) and Δ(λλλ) configurations. Moreover, a mirror plane passes through the tetracyanoplatinate anion (N1, C1, Pt, C2 and N2 atoms) and the [Ni(pn)3]2+ cation (Ni, C31 and C41 atoms). The coordination geometry around the NiII atom can be described as octahedral. The two N atoms occupying axial positions form an angle of 170.6 (4)° and the Ni—N bond distances range from 2.118 (9)–2.142 (10)Å [mean bond length is 2.131 (10) Å], in good agreement with the values reported of other [Ni(pn)3]2+ complexes (Behrens et al., 2003; Kuchár & Černák, 2008; Saha et al., 2005). Octahedral coordination geometry around the Ni atom was observed also in other compounds with [Ni(pn)3]2+ cation (Nasanen et al., 1964; Lin et al., 2005). The square-planar geometry of [Pt(CN)4]2- is in good agreement with those of the previous studies with average Pt—C bond lengths of 1.988 (10) Å. The structure is stabilized also by the N—H···N hydrogen bonds between the cations and anions (Table 2).