Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S010827010101294X/bj1030sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S010827010101294X/bj1030Isup2.hkl |
CCDC reference: 175063
For related literature, see: Alberti (1996); Benedetto et al. (1997); Clearfield (1988); Clearfield & Costantino (1996); Gunderman & Squattrito (1995); Kim & Lee (2000); Rogers et al. (1991); Suib (1993).
To an aqueous solution (50 ml) of NiCl2·6H2O (2.38 g, 10 mmol) was added p-toluenesulfonic acid (1.90 g, 10 mmol) with stirring at room temperature, followed by dropwise addition of neat propanediamine (0.74 g, 10 mmol). The resulting solution was kept in a refrigerator at 278 K. Blue block crystals of (I) suitable for X-ray analysis were obtained after a few weeks. Analysis calculated for C20H38N4O8S2Ni: C 41.04, H 6.54, N 9.57, O 21.86, S 10.96, Ni 10.03%; found: C 41.35, H 6.69, N 9.64, O 21.08, S 10.93, Ni 10.18%.
The H atoms of the water molecules were freely refined. All other H atoms were treated as riding, with C—H = 0.93–0.98 Å and N—H = 0.90 Å, and Uiso(H) = 1.2Ueq of the parent atom. Are these the correct constraints?
Data collection: XSCANS (Siemens, 1996); cell refinement: XSCANS; data reduction: SHELXTL (Siemens, 1997); program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.
[Ni(H2O)2(C3H10N2)2]2C7H7SO3 | ? # Insert any comments here. |
Mr = 585.37 | Dx = 1.395 Mg m−3 Dm = 1.40 Mg m−3 Dm measured by flotation in mesitylene-bromoform |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
a = 13.060 (2) Å | Cell parameters from 42 reflections |
b = 7.3266 (11) Å | θ = 5.4–12.5° |
c = 15.0029 (18) Å | µ = 0.89 mm−1 |
β = 103.842 (10)° | T = 295 K |
V = 1393.9 (3) Å3 | Block, blue |
Z = 2 | 0.40 × 0.32 × 0.23 mm |
F(000) = 620 |
Siemens P4 diffractometer | 2697 reflections with I > 2σ(I) |
Radiation source: fine-focus sealed tube | Rint = 0.028 |
Graphite monochromator | θmax = 27.5°, θmin = 2.8° |
ω/2θ scans | h = −16→1 |
Absorption correction: empirical (using intensity measurements) (North et al., 1968) | k = −9→1 |
Tmin = 0.280, Tmax = 0.339 | l = −19→19 |
4187 measured reflections | 3 standard reflections every 97 reflections |
3216 independent reflections | intensity decay: none |
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)] = 0.039 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.112 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.06 | w = 1/[σ2(Fo2) + (0.0577P)2 + 0.4802P] where P = (Fo2 + 2Fc2)/3 |
3216 reflections | (Δ/σ)max < 0.001 |
168 parameters | Δρmax = 0.73 e Å−3 |
2 restraints | Δρmin = −0.53 e Å−3 |
[Ni(H2O)2(C3H10N2)2]2C7H7SO3 | V = 1393.9 (3) Å3 |
Mr = 585.37 | Z = 2 |
Monoclinic, P21/c | Mo Kα radiation |
a = 13.060 (2) Å | µ = 0.89 mm−1 |
b = 7.3266 (11) Å | T = 295 K |
c = 15.0029 (18) Å | 0.40 × 0.32 × 0.23 mm |
β = 103.842 (10)° |
Siemens P4 diffractometer | 2697 reflections with I > 2σ(I) |
Absorption correction: empirical (using intensity measurements) (North et al., 1968) | Rint = 0.028 |
Tmin = 0.280, Tmax = 0.339 | 3 standard reflections every 97 reflections |
4187 measured reflections | intensity decay: none |
3216 independent reflections |
R[F2 > 2σ(F2)] = 0.039 | 2 restraints |
wR(F2) = 0.112 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.06 | Δρmax = 0.73 e Å−3 |
3216 reflections | Δρmin = −0.53 e Å−3 |
168 parameters |
Experimental. ? #Insert any special details here. |
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. |
x | y | z | Uiso*/Ueq | ||
Ni1 | 0.0000 | 0.0000 | 0.0000 | 0.03226 (12) | |
S1 | 0.18045 (4) | 0.13246 (9) | −0.27123 (3) | 0.04218 (16) | |
O1 | 0.1217 (2) | 0.0335 (4) | −0.34848 (17) | 0.0990 (10) | |
O2 | 0.12423 (15) | 0.1555 (3) | −0.20046 (13) | 0.0646 (5) | |
O3 | 0.21797 (17) | 0.3063 (3) | −0.29616 (18) | 0.0803 (7) | |
C1 | 0.29349 (18) | 0.0004 (3) | −0.22309 (15) | 0.0427 (5) | |
C2 | 0.3816 (2) | 0.0833 (5) | −0.1689 (2) | 0.0616 (7) | |
H2B | 0.3826 | 0.2086 | −0.1588 | 0.074* | |
C3 | 0.4684 (2) | −0.0228 (5) | −0.1297 (2) | 0.0740 (10) | |
H3B | 0.5279 | 0.0328 | −0.0934 | 0.089* | |
C4 | 0.4689 (2) | −0.2084 (5) | −0.1433 (2) | 0.0678 (9) | |
C5 | 0.3801 (2) | −0.2882 (5) | −0.1987 (2) | 0.0624 (7) | |
H5A | 0.3796 | −0.4132 | −0.2096 | 0.075* | |
C6 | 0.2921 (2) | −0.1851 (4) | −0.23830 (17) | 0.0504 (6) | |
H6A | 0.2327 | −0.2406 | −0.2748 | 0.061* | |
C7 | 0.5635 (3) | −0.3241 (7) | −0.0987 (3) | 0.1008 (14) | |
H7A | 0.6176 | −0.2475 | −0.0630 | 0.151* | |
H7B | 0.5898 | −0.3847 | −0.1454 | 0.151* | |
H7C | 0.5429 | −0.4134 | −0.0595 | 0.151* | |
N10 | −0.15659 (14) | −0.0601 (3) | 0.00195 (12) | 0.0406 (4) | |
H10A | −0.1867 | −0.1288 | −0.0471 | 0.049* | |
H10B | −0.1583 | −0.1230 | 0.0531 | 0.049* | |
N20 | −0.04730 (15) | 0.2643 (2) | 0.01926 (12) | 0.0386 (4) | |
H20A | 0.0043 | 0.3231 | 0.0596 | 0.046* | |
H20B | −0.0605 | 0.3255 | −0.0343 | 0.046* | |
C11 | −0.21463 (18) | 0.1131 (4) | −0.00016 (16) | 0.0476 (5) | |
H11A | −0.2755 | 0.0945 | 0.0252 | 0.057* | |
H11B | −0.2394 | 0.1539 | −0.0632 | 0.057* | |
C12 | −0.14405 (19) | 0.2568 (3) | 0.05474 (15) | 0.0446 (5) | |
H12A | −0.1238 | 0.2160 | 0.1188 | 0.053* | |
C13 | −0.1976 (3) | 0.4417 (5) | 0.0524 (2) | 0.0742 (9) | |
H13A | −0.1494 | 0.5274 | 0.0886 | 0.111* | |
H13B | −0.2588 | 0.4302 | 0.0770 | 0.111* | |
H13C | −0.2186 | 0.4842 | −0.0098 | 0.111* | |
O30 | −0.05333 (14) | 0.0500 (3) | −0.14507 (11) | 0.0455 (4) | |
H30A | −0.008 (2) | 0.069 (5) | −0.181 (2) | 0.070 (9)* | |
H30B | −0.103 (2) | −0.021 (4) | −0.180 (2) | 0.086 (12)* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Ni1 | 0.0353 (2) | 0.0332 (2) | 0.02864 (19) | −0.00217 (14) | 0.00832 (13) | 0.00087 (14) |
S1 | 0.0463 (3) | 0.0521 (3) | 0.0276 (2) | 0.0085 (2) | 0.0078 (2) | 0.0040 (2) |
O1 | 0.0992 (18) | 0.104 (2) | 0.0644 (14) | 0.0497 (15) | −0.0380 (13) | −0.0361 (13) |
O2 | 0.0602 (11) | 0.0904 (15) | 0.0500 (10) | 0.0144 (11) | 0.0267 (8) | 0.0151 (10) |
O3 | 0.0664 (13) | 0.0778 (15) | 0.1020 (17) | 0.0139 (11) | 0.0308 (12) | 0.0482 (14) |
C1 | 0.0421 (11) | 0.0539 (13) | 0.0314 (9) | 0.0054 (10) | 0.0075 (8) | 0.0069 (9) |
C2 | 0.0575 (15) | 0.0607 (17) | 0.0584 (15) | −0.0028 (14) | −0.0020 (12) | 0.0084 (14) |
C3 | 0.0457 (15) | 0.096 (3) | 0.0697 (19) | −0.0071 (15) | −0.0063 (13) | 0.0155 (17) |
C4 | 0.0476 (14) | 0.101 (3) | 0.0573 (15) | 0.0220 (16) | 0.0178 (12) | 0.0267 (16) |
C5 | 0.0666 (17) | 0.0630 (17) | 0.0612 (16) | 0.0190 (14) | 0.0225 (13) | 0.0088 (14) |
C6 | 0.0516 (13) | 0.0559 (15) | 0.0436 (12) | 0.0064 (11) | 0.0108 (10) | 0.0019 (11) |
C7 | 0.0645 (19) | 0.150 (4) | 0.089 (2) | 0.048 (2) | 0.0205 (18) | 0.044 (3) |
N10 | 0.0404 (9) | 0.0458 (10) | 0.0358 (9) | −0.0068 (8) | 0.0097 (7) | 0.0011 (8) |
N20 | 0.0458 (10) | 0.0370 (9) | 0.0315 (8) | −0.0010 (8) | 0.0059 (7) | 0.0028 (7) |
C11 | 0.0392 (11) | 0.0602 (15) | 0.0450 (12) | 0.0042 (11) | 0.0132 (9) | 0.0095 (11) |
C12 | 0.0567 (13) | 0.0436 (12) | 0.0365 (10) | 0.0091 (10) | 0.0170 (9) | 0.0061 (9) |
C13 | 0.099 (2) | 0.0563 (16) | 0.080 (2) | 0.0280 (18) | 0.0457 (19) | 0.0127 (16) |
O30 | 0.0512 (9) | 0.0521 (9) | 0.0326 (7) | −0.0056 (8) | 0.0090 (7) | 0.0027 (7) |
Ni1—N20 | 2.0736 (18) | C6—H6A | 0.9300 |
Ni1—N20i | 2.0736 (18) | C7—H7A | 0.9600 |
Ni1—N10i | 2.0991 (18) | C7—H7B | 0.9600 |
Ni1—N10 | 2.0991 (18) | C7—H7C | 0.9600 |
Ni1—O30 | 2.1521 (16) | N10—C11 | 1.475 (3) |
Ni1—O30i | 2.1521 (16) | N10—H10A | 0.9000 |
S1—O1 | 1.426 (2) | N10—H10B | 0.9000 |
S1—O2 | 1.4380 (18) | N20—C12 | 1.485 (3) |
S1—O3 | 1.446 (2) | N20—H20A | 0.9000 |
S1—C1 | 1.768 (2) | N20—H20B | 0.9000 |
C1—C6 | 1.378 (4) | C11—C12 | 1.507 (4) |
C1—C2 | 1.381 (4) | C11—H11A | 0.9700 |
C2—C3 | 1.385 (4) | C11—H11B | 0.9700 |
C2—H2B | 0.9300 | C12—C13 | 1.522 (4) |
C3—C4 | 1.375 (5) | C12—H12A | 0.9800 |
C3—H3B | 0.9300 | C13—H13A | 0.9600 |
C4—C5 | 1.384 (5) | C13—H13B | 0.9600 |
C4—C7 | 1.516 (4) | C13—H13C | 0.9600 |
C5—C6 | 1.385 (4) | O30—H30A | 0.902 (18) |
C5—H5A | 0.9300 | O30—H30B | 0.893 (18) |
N20—Ni1—N20i | 180.00 (12) | C4—C7—H7A | 109.5 |
N20—Ni1—N10i | 97.46 (8) | C4—C7—H7B | 109.5 |
N20i—Ni1—N10i | 82.54 (8) | H7A—C7—H7B | 109.5 |
N20—Ni1—N10 | 82.54 (8) | C4—C7—H7C | 109.5 |
N20i—Ni1—N10 | 97.46 (8) | H7A—C7—H7C | 109.5 |
N10i—Ni1—N10 | 180.00 (10) | H7B—C7—H7C | 109.5 |
N20—Ni1—O30 | 86.95 (7) | C11—N10—Ni1 | 108.46 (14) |
N20i—Ni1—O30 | 93.05 (7) | C11—N10—H10A | 110.0 |
N10i—Ni1—O30 | 91.77 (7) | Ni1—N10—H10A | 110.0 |
N10—Ni1—O30 | 88.23 (7) | C11—N10—H10B | 110.0 |
N20—Ni1—O30i | 93.05 (7) | Ni1—N10—H10B | 110.0 |
N20i—Ni1—O30i | 86.95 (7) | H10A—N10—H10B | 108.4 |
N10i—Ni1—O30i | 88.23 (7) | C12—N20—Ni1 | 108.83 (13) |
N10—Ni1—O30i | 91.77 (7) | C12—N20—H20A | 109.9 |
O30—Ni1—O30i | 180.00 (3) | Ni1—N20—H20A | 109.9 |
O1—S1—O2 | 112.91 (18) | C12—N20—H20B | 109.9 |
O1—S1—O3 | 112.81 (19) | Ni1—N20—H20B | 109.9 |
O2—S1—O3 | 110.62 (15) | H20A—N20—H20B | 108.3 |
O1—S1—C1 | 106.75 (13) | N10—C11—C12 | 110.20 (18) |
O2—S1—C1 | 106.65 (11) | N10—C11—H11A | 109.6 |
O3—S1—C1 | 106.63 (12) | C12—C11—H11A | 109.6 |
C6—C1—C2 | 120.5 (2) | N10—C11—H11B | 109.6 |
C6—C1—S1 | 119.7 (2) | C12—C11—H11B | 109.6 |
C2—C1—S1 | 119.8 (2) | H11A—C11—H11B | 108.1 |
C1—C2—C3 | 119.0 (3) | N20—C12—C11 | 106.95 (18) |
C1—C2—H2B | 120.5 | N20—C12—C13 | 112.6 (2) |
C3—C2—H2B | 120.5 | C11—C12—C13 | 113.0 (2) |
C4—C3—C2 | 121.7 (3) | N20—C12—H12A | 108.0 |
C4—C3—H3B | 119.2 | C11—C12—H12A | 108.0 |
C2—C3—H3B | 119.2 | C13—C12—H12A | 108.0 |
C3—C4—C5 | 118.3 (3) | C12—C13—H13A | 109.5 |
C3—C4—C7 | 121.3 (4) | C12—C13—H13B | 109.5 |
C5—C4—C7 | 120.4 (4) | H13A—C13—H13B | 109.5 |
C4—C5—C6 | 121.1 (3) | C12—C13—H13C | 109.5 |
C4—C5—H5A | 119.4 | H13A—C13—H13C | 109.5 |
C6—C5—H5A | 119.4 | H13B—C13—H13C | 109.5 |
C1—C6—C5 | 119.4 (3) | Ni1—O30—H30A | 122 (2) |
C1—C6—H6A | 120.3 | Ni1—O30—H30B | 120 (3) |
C5—C6—H6A | 120.3 | H30A—O30—H30B | 103 (3) |
O1—S1—C1—C6 | −23.5 (3) | C4—C5—C6—C1 | 0.8 (4) |
O2—S1—C1—C6 | 97.4 (2) | N20—Ni1—N10—C11 | 9.26 (13) |
O3—S1—C1—C6 | −144.3 (2) | N20i—Ni1—N10—C11 | −170.74 (13) |
O1—S1—C1—C2 | 157.9 (3) | O30—Ni1—N10—C11 | −77.90 (14) |
O2—S1—C1—C2 | −81.1 (2) | O30i—Ni1—N10—C11 | 102.10 (14) |
O3—S1—C1—C2 | 37.1 (2) | N10i—Ni1—N20—C12 | −160.83 (14) |
C6—C1—C2—C3 | −0.2 (4) | N10—Ni1—N20—C12 | 19.17 (14) |
S1—C1—C2—C3 | 178.3 (2) | O30—Ni1—N20—C12 | 107.79 (14) |
C1—C2—C3—C4 | −0.2 (5) | O30i—Ni1—N20—C12 | −72.21 (14) |
C2—C3—C4—C5 | 0.9 (5) | Ni1—N10—C11—C12 | −36.2 (2) |
C2—C3—C4—C7 | −178.8 (3) | Ni1—N20—C12—C11 | −43.32 (19) |
C3—C4—C5—C6 | −1.2 (4) | Ni1—N20—C12—C13 | −168.1 (2) |
C7—C4—C5—C6 | 178.5 (3) | N10—C11—C12—N20 | 53.2 (2) |
C2—C1—C6—C5 | 0.0 (4) | N10—C11—C12—C13 | 177.7 (2) |
S1—C1—C6—C5 | −178.59 (19) |
Symmetry code: (i) −x, −y, −z. |
D—H···A | D—H | H···A | D···A | D—H···A |
N10—H10A···O3ii | 0.90 | 2.34 | 3.154 (3) | 151 |
N10—H10B···O2i | 0.90 | 2.16 | 2.989 (3) | 153 |
N20—H20A···O1iii | 0.90 | 2.08 | 2.984 (3) | 178 |
N20—H20A···S1iii | 0.90 | 3.01 | 3.8505 (19) | 157 |
N20—H20B···O1iv | 0.90 | 2.32 | 3.195 (3) | 164 |
O30—H30A···O2 | 0.90 (2) | 1.93 (2) | 2.755 (3) | 151 (3) |
O30—H30B···O3ii | 0.89 (2) | 1.93 (2) | 2.772 (3) | 156 (4) |
O30—H30B···S1ii | 0.89 (2) | 2.77 (2) | 3.563 (2) | 149 (3) |
Symmetry codes: (i) −x, −y, −z; (ii) −x, y−1/2, −z−1/2; (iii) x, −y+1/2, z+1/2; (iv) −x, y+1/2, −z−1/2. |
Experimental details
Crystal data | |
Chemical formula | [Ni(H2O)2(C3H10N2)2]2C7H7SO3 |
Mr | 585.37 |
Crystal system, space group | Monoclinic, P21/c |
Temperature (K) | 295 |
a, b, c (Å) | 13.060 (2), 7.3266 (11), 15.0029 (18) |
β (°) | 103.842 (10) |
V (Å3) | 1393.9 (3) |
Z | 2 |
Radiation type | Mo Kα |
µ (mm−1) | 0.89 |
Crystal size (mm) | 0.40 × 0.32 × 0.23 |
Data collection | |
Diffractometer | Siemens P4 diffractometer |
Absorption correction | Empirical (using intensity measurements) (North et al., 1968) |
Tmin, Tmax | 0.280, 0.339 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 4187, 3216, 2697 |
Rint | 0.028 |
(sin θ/λ)max (Å−1) | 0.650 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.039, 0.112, 1.06 |
No. of reflections | 3216 |
No. of parameters | 168 |
No. of restraints | 2 |
H-atom treatment | H atoms treated by a mixture of independent and constrained refinement |
Δρmax, Δρmin (e Å−3) | 0.73, −0.53 |
Computer programs: XSCANS (Siemens, 1996), XSCANS, SHELXTL (Siemens, 1997), SHELXS97 (Sheldrick, 1990), SHELXL97 (Sheldrick, 1997), SHELXTL.
D—H···A | D—H | H···A | D···A | D—H···A |
N10—H10A···O3i | 0.90 | 2.34 | 3.154 (3) | 151 |
N10—H10B···O2ii | 0.90 | 2.16 | 2.989 (3) | 153 |
N20—H20A···O1iii | 0.90 | 2.08 | 2.984 (3) | 178 |
N20—H20B···O1iv | 0.90 | 2.32 | 3.195 (3) | 164 |
O30—H30A···O2 | 0.902 (18) | 1.93 (2) | 2.755 (3) | 151 (3) |
O30—H30B···O3i | 0.893 (18) | 1.93 (2) | 2.772 (3) | 156 (4) |
Symmetry codes: (i) −x, y−1/2, −z−1/2; (ii) −x, −y, −z; (iii) x, −y+1/2, z+1/2; (iv) −x, y+1/2, −z−1/2. |
Subscribe to Acta Crystallographica Section C: Structural Chemistry
The full text of this article is available to subscribers to the journal.
- Information on subscribing
- Sample issue
- Purchase subscription
- Reduced-price subscriptions
- If you have already subscribed, you may need to register
Compounds forming layered structures have been of great interest in both academic research and industrial applications, because of their possible use as ion exchangers and intercalation materials (Clearfield, 1988; Suib, 1993). Particularly, metal phosphate and phosphonate compounds, such as zirconium and titanium phosphates and phosphonates, have been extensively studied as a new family of layered materials (Clearfield & Costantino, 1996; Alberti, 1996). Most commonly, these mixed inorganic-organic two-dimensional compounds contain covalent metal-oxygen-phosphorus frameworks. In recent years, Squattrito and co-workers have studied metal organosulfonate compounds (Gunderman & Squattrito, 1995; Benedetto et al., 1997), and they have reported two-dimensional materials with layered structures analogous to the recently reported metal phosphonate structures. In our group, research has been directed towards the development of new layered and porous materials (Kim & Lee, 2000), using weaker metal sulfonate interactions. This approach takes advantage of the flexible coordination behaviour of the SO3- group to obtain structures. In this paper, we report the preparation and crystal structure of the title nickel(II) sulfonate complex, (I), which is chelated by propanediamine ligands. \sch
As shown in Fig 1, the NiII cation of (I) lies on a crystallographic inversion centre and is six-coordinate, with two propanediamine ligands attached at the equatorial positions and two water molecules at the axial positions. Its coordination geometry can be described as a slightly distorted octahedral arrangement. The Ni—N distances range from 2.074 (2) to 2.099 (2) Å and the Ni—O distance is 2.152 (2) Å. The inter-ligand N—Ni—N angle is 82.54 (8)° and the N—Ni—O angles are in the range 86.95 (7)–88.23 (7)°.
The S—Osulfonate bond lengths in the p-toluenesulfonate anion range from 1.426 (2) to 1.446 (2) Å and the S—C bond length is 1.768 (2) Å. The Osulfonate—S—Osulfonate and Osulfonate—S—C bond angles are in the range 110.6 (2) to 112.9 (2)° and 106.6 (1) to 106.8 (1)°, respectively. The geometrical data for this anion are consistent with those previously reported by Rogers et al. (1991).
As shown in Fig. 2, compound (I) forms a layered structure consisting of dicationic [Ni(H2O)2{NH2CH2CH(NH2)CH3}2]2+ layers and anionic CH3C6H4SO3- layers. The arrangement of the p-toluenesulfonate anions has the sulfonate groups turned alternately toward opposite sides of the layers. The water molecules coordinated to the NiII cations and most of the O atoms of the p-toluenesulfonate anions are linked together in hydrogen-bonded chains along [001], with strong Owater—H···Osulfonate hydrogen bonds (O30—H30A···O2 and O30—H30B···O3; Table 1). These chains are cross-linked in the (011) plane by the Ndiamine—H···Osulfonate hydrogen-bonding interactions formed between the amine H atoms of the propanediamine ligands and the sulfonate O atoms of the p-toluenesulfonate anions (N20—H20A···O1, N20—H20B···O1, N10—H10B···O2 and N10—H10A···O3; Table 1). Thus, all hydrogen bonds are formed by contacts between cations and anions, and so all contribute to the stabilization of the crystal structure.
In conclusion, the crystal structure of (I) consists of a highly layered two-dimensional network, with hydrophilic and hydrophobic sections alternating along [100]. The crystal structure is stabilized through hydrogen bonding. There is no direct bonding between the NiII cation and the sulfonate O atoms of the anion. Therefore, this NiII sulfonate compound is quite different in structure from the reported metal phosphonates (Clearfield & Costantino, 1996; Alberti, 1996).