Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270102010764/sk1555sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108270102010764/sk1555Isup2.hkl |
CCDC reference: 193400
Nickel chloride hexahydrate (0.476 g, 2 mmol) was dissolved in a mixture of water, methanol and acetone (3:2:2). The resulting clear green solution was reacted with a solution of bis(tetra-n-butylammonium) bis(2-thioxo-1,3-dithiole-4,5-dithiolato)zincate(II) [1.88 g, 2 mmol; prepared according to the method of Valade et al. (1985)] in acetone for several days or longer, until all the solvents except water had evaporated completely. The resulting mixture was filtered to give a green-black solid, and this solid was then redissolved in acetone to recrystallize. After several days, the solvent was evaporated off to give shiny stick-like green-black crystals of (I).
After checking their presence in the difference map, all H atoms were geometrically fixed and allowed to ride on their attached atoms, with C—H = 0.96–0.97 Å and Uiso(H) = 1.2Ueq(C).
Data collection: XSCANS (Siemens, 1996); cell refinement: XSCANS; data reduction: XSCANS; program(s) used to solve structure: SHELXTL (Bruker, 1997); program(s) used to refine structure: SHELXTL; molecular graphics: PLATON (Spek, 2001).
(C16H36N)[Ni(C3S5)2] | F(000) = 1452 |
Mr = 693.91 | Dx = 1.456 Mg m−3 |
Monoclinic, C2/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -C 2yc | Cell parameters from 32 reflections |
a = 20.191 (2) Å | θ = 5.1–12.5° |
b = 13.4041 (14) Å | µ = 1.29 mm−1 |
c = 12.1408 (14) Å | T = 293 K |
β = 105.554 (8)° | Prism, black |
V = 3165.5 (6) Å3 | 0.38 × 0.30 × 0.20 mm |
Z = 4 |
Bruker P4 diffractometer | 1834 reflections with I > 2σ(I) |
Radiation source: fine-focus sealed tube | Rint = 0.028 |
Graphite monochromator | θmax = 25.0°, θmin = 1.9° |
θ/2θ scans | h = −1→24 |
Absorption correction: ψ scan (XSCANS; Siemens, 1996) | k = −1→15 |
Tmin = 0.636, Tmax = 0.773 | l = −14→14 |
3338 measured reflections | 3 standard reflections every 97 reflections |
2791 independent reflections | intensity decay: 1% |
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)] = 0.059 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.157 | H-atom parameters constrained |
S = 1.12 | w = 1/[σ2(Fo2) + (0.0504P)2 + 7.7955P] where P = (Fo2 + 2Fc2)/3 |
2789 reflections | (Δ/σ)max < 0.001 |
155 parameters | Δρmax = 0.74 e Å−3 |
7 restraints | Δρmin = −0.53 e Å−3 |
(C16H36N)[Ni(C3S5)2] | V = 3165.5 (6) Å3 |
Mr = 693.91 | Z = 4 |
Monoclinic, C2/c | Mo Kα radiation |
a = 20.191 (2) Å | µ = 1.29 mm−1 |
b = 13.4041 (14) Å | T = 293 K |
c = 12.1408 (14) Å | 0.38 × 0.30 × 0.20 mm |
β = 105.554 (8)° |
Bruker P4 diffractometer | 1834 reflections with I > 2σ(I) |
Absorption correction: ψ scan (XSCANS; Siemens, 1996) | Rint = 0.028 |
Tmin = 0.636, Tmax = 0.773 | 3 standard reflections every 97 reflections |
3338 measured reflections | intensity decay: 1% |
2791 independent reflections |
R[F2 > 2σ(F2)] = 0.059 | 7 restraints |
wR(F2) = 0.157 | H-atom parameters constrained |
S = 1.12 | Δρmax = 0.74 e Å−3 |
2789 reflections | Δρmin = −0.53 e Å−3 |
155 parameters |
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 | Occ. (<1) | |
Ni1 | 0.0000 | 0.0000 | 0.0000 | 0.0618 (3) | |
S1 | −0.34892 (9) | 0.09595 (18) | −0.0172 (2) | 0.1137 (7) | |
S2 | −0.20012 (8) | 0.12642 (14) | 0.08469 (16) | 0.0902 (6) | |
S3 | −0.24403 (8) | 0.00017 (14) | −0.11304 (15) | 0.0826 (5) | |
S4 | −0.04975 (8) | 0.08814 (13) | 0.10294 (14) | 0.0818 (5) | |
N1 | −0.5000 | 0.2118 (4) | 0.2500 | 0.0556 (14) | |
C1 | −0.2684 (3) | 0.0754 (5) | −0.0147 (6) | 0.0815 (18) | |
C2 | −0.1348 (3) | 0.0708 (4) | 0.0364 (5) | 0.0690 (15) | |
C3 | −0.1553 (3) | 0.0127 (4) | −0.0565 (5) | 0.0666 (14) | |
C4 | −0.5111 (3) | 0.1444 (4) | 0.1458 (4) | 0.0663 (15) | |
H4A | −0.4700 | 0.1047 | 0.1534 | 0.080* | |
H4B | −0.5484 | 0.0988 | 0.1459 | 0.080* | |
C5 | −0.5274 (4) | 0.1962 (6) | 0.0327 (5) | 0.107 (2) | |
H5A | −0.4884 | 0.2364 | 0.0279 | 0.129* | |
H5B | −0.5663 | 0.2405 | 0.0263 | 0.129* | |
C6 | −0.5442 (4) | 0.1224 (7) | −0.0651 (5) | 0.124 (3) | |
H6A | −0.5785 | 0.0763 | −0.0525 | 0.149* | |
H6B | −0.5031 | 0.0841 | −0.0627 | 0.149* | |
C7 | −0.5707 (6) | 0.1660 (8) | −0.1842 (6) | 0.194 (5) | |
H7A | −0.5795 | 0.1130 | −0.2395 | 0.292* | |
H7B | −0.5368 | 0.2103 | −0.1993 | 0.292* | |
H7C | −0.6124 | 0.2021 | −0.1893 | 0.292* | |
C8 | −0.5613 (3) | 0.2787 (5) | 0.2402 (5) | 0.0813 (18) | |
H8A | −0.5644 | 0.3246 | 0.1772 | 0.098* | |
H8B | −0.5536 | 0.3181 | 0.3095 | 0.098* | |
C9 | −0.6299 (3) | 0.2248 (6) | 0.2212 (6) | 0.115 (3) | |
H9A | −0.6362 | 0.1957 | 0.2909 | 0.138* | |
H9B | −0.6367 | 0.1744 | 0.1618 | 0.138* | |
C10 | −0.6752 (4) | 0.3177 (6) | 0.1828 (13) | 0.109 (5)* | 0.533 (12) |
H10A | −0.6608 | 0.3703 | 0.2389 | 0.131* | 0.533 (12) |
H10B | −0.6692 | 0.3415 | 0.1106 | 0.131* | 0.533 (12) |
C11 | −0.7516 (4) | 0.2936 (10) | 0.1688 (12) | 0.114 (6)* | 0.533 (12) |
H11A | −0.7775 | 0.3545 | 0.1593 | 0.172* | 0.533 (12) |
H11B | −0.7564 | 0.2593 | 0.2356 | 0.172* | 0.533 (12) |
H11C | −0.7684 | 0.2521 | 0.1028 | 0.172* | 0.533 (12) |
C10' | −0.6963 (5) | 0.2767 (8) | 0.2300 (10) | 0.083 (5)* | 0.467 (12) |
H10C | −0.6895 | 0.3065 | 0.3050 | 0.100* | 0.467 (12) |
H10D | −0.7335 | 0.2287 | 0.2186 | 0.100* | 0.467 (12) |
C11' | −0.7140 (7) | 0.3579 (9) | 0.1369 (11) | 0.102 (6)* | 0.467 (12) |
H11D | −0.7547 | 0.3928 | 0.1416 | 0.154* | 0.467 (12) |
H11E | −0.7219 | 0.3273 | 0.0629 | 0.154* | 0.467 (12) |
H11F | −0.6764 | 0.4040 | 0.1480 | 0.154* | 0.467 (12) |
S5 | −0.09697 (7) | −0.04710 (13) | −0.11339 (14) | 0.0780 (5) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Ni1 | 0.0574 (6) | 0.0608 (6) | 0.0729 (6) | −0.0082 (5) | 0.0274 (5) | −0.0046 (5) |
S1 | 0.0636 (10) | 0.1463 (19) | 0.1424 (18) | 0.0031 (11) | 0.0469 (11) | 0.0059 (15) |
S2 | 0.0675 (10) | 0.1020 (13) | 0.1129 (13) | −0.0050 (9) | 0.0448 (9) | −0.0224 (11) |
S3 | 0.0576 (8) | 0.0922 (11) | 0.0994 (12) | −0.0109 (8) | 0.0233 (8) | −0.0052 (10) |
S4 | 0.0620 (9) | 0.0960 (12) | 0.0940 (11) | −0.0151 (8) | 0.0323 (8) | −0.0321 (9) |
N1 | 0.062 (4) | 0.049 (3) | 0.060 (3) | 0.000 | 0.022 (3) | 0.000 |
C1 | 0.067 (4) | 0.085 (4) | 0.104 (5) | −0.005 (3) | 0.041 (3) | 0.016 (4) |
C2 | 0.057 (3) | 0.072 (4) | 0.087 (4) | −0.008 (3) | 0.036 (3) | −0.005 (3) |
C3 | 0.062 (3) | 0.060 (3) | 0.085 (4) | −0.008 (3) | 0.032 (3) | 0.001 (3) |
C4 | 0.086 (4) | 0.061 (3) | 0.056 (3) | 0.014 (3) | 0.024 (3) | −0.002 (3) |
C5 | 0.143 (7) | 0.124 (6) | 0.063 (4) | 0.032 (5) | 0.041 (4) | 0.019 (4) |
C6 | 0.143 (7) | 0.170 (8) | 0.062 (4) | 0.031 (6) | 0.032 (5) | −0.013 (5) |
C7 | 0.277 (14) | 0.168 (10) | 0.101 (7) | −0.041 (10) | −0.014 (8) | −0.015 (7) |
C8 | 0.077 (4) | 0.081 (4) | 0.082 (4) | 0.016 (3) | 0.014 (3) | −0.025 (3) |
C9 | 0.067 (4) | 0.174 (8) | 0.107 (5) | 0.010 (5) | 0.029 (4) | −0.028 (6) |
S5 | 0.0618 (9) | 0.0860 (11) | 0.0878 (11) | −0.0052 (8) | 0.0228 (8) | −0.0220 (9) |
Ni1—S4 | 2.1541 (15) | C6—H6B | 0.9700 |
Ni1—S4i | 2.1541 (15) | C7—H7A | 0.9600 |
Ni1—S5 | 2.1638 (15) | C7—H7B | 0.9600 |
Ni1—S5i | 2.1638 (15) | C7—H7C | 0.9600 |
S1—C1 | 1.642 (6) | C8—C9 | 1.525 (8) |
S2—C1 | 1.712 (7) | C8—H8A | 0.9700 |
S2—C2 | 1.748 (5) | C8—H8B | 0.9700 |
S3—C1 | 1.732 (7) | C9—C10' | 1.5394 (10) |
S3—C3 | 1.747 (6) | C9—C10 | 1.5410 (10) |
S4—C2 | 1.706 (6) | C9—H9A | 0.9700 |
N1—C8ii | 1.507 (6) | C9—H9B | 0.9700 |
N1—C8 | 1.507 (6) | C10—C11 | 1.5396 (11) |
N1—C4 | 1.521 (6) | C10—H10A | 0.9700 |
N1—C4ii | 1.521 (6) | C10—H10B | 0.9700 |
C2—C3 | 1.341 (8) | C11—H11A | 0.9600 |
C3—S5 | 1.715 (6) | C11—H11B | 0.9600 |
C4—C5 | 1.494 (7) | C11—H11C | 0.9600 |
C4—H4A | 0.9700 | C10'—C11' | 1.5403 (10) |
C4—H4B | 0.9700 | C10'—H10C | 0.9700 |
C5—C6 | 1.512 (9) | C10'—H10D | 0.9700 |
C5—H5A | 0.9700 | C11'—H11D | 0.9600 |
C5—H5B | 0.9700 | C11'—H11E | 0.9600 |
C6—C7 | 1.517 (5) | C11'—H11F | 0.9600 |
C6—H6A | 0.9700 | ||
S4—Ni1—S4i | 180.00 (11) | H7A—C7—H7B | 109.5 |
S4—Ni1—S5 | 92.63 (6) | C6—C7—H7C | 109.5 |
S4i—Ni1—S5 | 87.37 (6) | H7A—C7—H7C | 109.5 |
S4—Ni1—S5i | 87.37 (6) | H7B—C7—H7C | 109.5 |
S4i—Ni1—S5i | 92.63 (6) | N1—C8—C9 | 115.0 (5) |
S5—Ni1—S5i | 180.00 (11) | N1—C8—H8A | 108.5 |
C1—S2—C2 | 97.5 (3) | C9—C8—H8A | 108.5 |
C1—S3—C3 | 97.1 (3) | N1—C8—H8B | 108.5 |
C2—S4—Ni1 | 102.5 (2) | C9—C8—H8B | 108.5 |
C8ii—N1—C8 | 106.9 (6) | H8A—C8—H8B | 107.5 |
C8ii—N1—C4 | 110.7 (3) | C8—C9—C10' | 123.2 (7) |
C8—N1—C4 | 110.6 (3) | C8—C9—C10 | 95.9 (6) |
C8ii—N1—C4ii | 110.6 (3) | C8—C9—H9A | 112.6 |
C8—N1—C4ii | 110.7 (3) | C10'—C9—H9A | 78.6 |
C4—N1—C4ii | 107.2 (5) | C10—C9—H9A | 112.6 |
S1—C1—S2 | 123.5 (4) | C8—C9—H9B | 112.6 |
S1—C1—S3 | 123.2 (4) | C10'—C9—H9B | 114.5 |
S2—C1—S3 | 113.3 (3) | C10—C9—H9B | 112.6 |
C3—C2—S4 | 121.4 (4) | H9A—C9—H9B | 110.1 |
C3—C2—S2 | 116.1 (4) | C11—C10—C9 | 111.0 (3) |
S4—C2—S2 | 122.5 (4) | C11—C10—H10A | 109.4 |
C2—C3—S5 | 121.3 (4) | C9—C10—H10A | 109.4 |
C2—C3—S3 | 116.0 (4) | C11—C10—H10B | 109.4 |
S5—C3—S3 | 122.6 (4) | C9—C10—H10B | 109.4 |
C5—C4—N1 | 115.8 (5) | H10A—C10—H10B | 108.0 |
C5—C4—H4A | 108.3 | C10—C11—H11A | 109.5 |
N1—C4—H4A | 108.3 | C10—C11—H11B | 109.5 |
C5—C4—H4B | 108.3 | H11A—C11—H11B | 109.5 |
N1—C4—H4B | 108.3 | C10—C11—H11C | 109.5 |
H4A—C4—H4B | 107.4 | H11A—C11—H11C | 109.5 |
C4—C5—C6 | 111.5 (6) | H11B—C11—H11C | 109.5 |
C4—C5—H5A | 109.3 | C9—C10'—C11' | 107.6 (3) |
C6—C5—H5A | 109.3 | C9—C10'—H10C | 110.2 |
C4—C5—H5B | 109.3 | C11'—C10'—H10C | 110.2 |
C6—C5—H5B | 109.3 | C9—C10'—H10D | 110.2 |
H5A—C5—H5B | 108.0 | C11'—C10'—H10D | 110.2 |
C5—C6—C7 | 116.4 (7) | H10C—C10'—H10D | 108.5 |
C5—C6—H6A | 108.2 | C10'—C11'—H11D | 109.5 |
C7—C6—H6A | 108.2 | C10'—C11'—H11E | 109.5 |
C5—C6—H6B | 108.2 | H11D—C11'—H11E | 109.5 |
C7—C6—H6B | 108.2 | C10'—C11'—H11F | 109.5 |
H6A—C6—H6B | 107.3 | H11D—C11'—H11F | 109.5 |
C6—C7—H7A | 109.5 | H11E—C11'—H11F | 109.5 |
C6—C7—H7B | 109.5 | C3—S5—Ni1 | 102.1 (2) |
Symmetry codes: (i) −x, −y, −z; (ii) −x−1, y, −z+1/2. |
Experimental details
Crystal data | |
Chemical formula | (C16H36N)[Ni(C3S5)2] |
Mr | 693.91 |
Crystal system, space group | Monoclinic, C2/c |
Temperature (K) | 293 |
a, b, c (Å) | 20.191 (2), 13.4041 (14), 12.1408 (14) |
β (°) | 105.554 (8) |
V (Å3) | 3165.5 (6) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 1.29 |
Crystal size (mm) | 0.38 × 0.30 × 0.20 |
Data collection | |
Diffractometer | Bruker P4 diffractometer |
Absorption correction | ψ scan (XSCANS; Siemens, 1996) |
Tmin, Tmax | 0.636, 0.773 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 3338, 2791, 1834 |
Rint | 0.028 |
(sin θ/λ)max (Å−1) | 0.594 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.059, 0.157, 1.12 |
No. of reflections | 2789 |
No. of parameters | 155 |
No. of restraints | 7 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 0.74, −0.53 |
Computer programs: XSCANS (Siemens, 1996), XSCANS, SHELXTL (Bruker, 1997), SHELXTL, PLATON (Spek, 2001).
Ni1—S4 | 2.1541 (15) | S3—C1 | 1.732 (7) |
Ni1—S5 | 2.1638 (15) | S3—C3 | 1.747 (6) |
S1—C1 | 1.642 (6) | S4—C2 | 1.706 (6) |
S2—C1 | 1.712 (7) | C2—C3 | 1.341 (8) |
S2—C2 | 1.748 (5) | C3—S5 | 1.715 (6) |
S4—Ni1—S4i | 180.00 (11) | S1—C1—S2 | 123.5 (4) |
S4—Ni1—S5 | 92.63 (6) | S1—C1—S3 | 123.2 (4) |
S4i—Ni1—S5 | 87.37 (6) | S2—C1—S3 | 113.3 (3) |
S4—Ni1—S5i | 87.37 (6) | C3—C2—S4 | 121.4 (4) |
S4i—Ni1—S5i | 92.63 (6) | C3—C2—S2 | 116.1 (4) |
S5—Ni1—S5i | 180.00 (11) | S4—C2—S2 | 122.5 (4) |
C1—S2—C2 | 97.5 (3) | C2—C3—S5 | 121.3 (4) |
C1—S3—C3 | 97.1 (3) | C2—C3—S3 | 116.0 (4) |
C2—S4—Ni1 | 102.5 (2) | S5—C3—S3 | 122.6 (4) |
Symmetry code: (i) −x, −y, −z. |
No. | 1a | 2b | 3c | 4d | |
Space group | P1 | P21/c | P1 | C2/c | |
Cell | a | 12.144 | 14.649 (3) | 11.702 (2) | 20.191 (2) |
parameters | b | 12.161 | 13.497 (3) | 12.120 (2) | 13.4041 (14) |
(Å, °) | c | 12.173 | 16.383 (4) | 12.358 (2) | 12.1408 (14) |
α | 77.02 | 90 | 100.04 (1) | 90 | |
β | 102.95 | 91.14 (6) | 91.93 (1) | 105.554 (8) | |
γ | 112.88 | 90 | 105.44 (1) | 90 | |
Volume (Å3) | 1595.1 | 3238.6 | 1657.6 | 3165.5 (6) | |
Density (Mg m-3) | 1.444 | 1.423 | 1.39 | 1.456 | |
Temperature (K) | 295 | 295 | 295 | 293 (2) | |
R-factor (%) | 0.0 | 5.4 | 3.66 | 5.5 |
Notes: (a) Sjolin et al. (1977); (b) Lindqvist et al. (1982); (c) Mentzafos et al. (1988); (d) this work. |
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Nickel complexes of 4,5-dimercapto-1,3-dithiole-2-thione (dmit) and their π-conjugation-extended derivatives have received steady interest in the field of molecular conductors (Lei et al., 1996; Narvor et al., 1996; Tanaka et al., 2001). Recently, the title compound, (I), was synthesized using a more direct method (see Experimental), instead of the commonly used dibenzoyl derivative of dmit (Valade et al., 1985, and references therein). It was also found that several different crystal structures of (I) have been reported (Table 2). Thus, it was postulated that compound (I) synthesized using the direct method might crystallize in a new structure, and this was the first reason for the present determination of (I). Another reason is due to the fact that the fluorescence emission spectra of (I) and the analogous bis(tetra-n-butylammonium) bis(2-thioxo-1,3-dithiole-4,5-dithiolato)zincate(II) have recently been measured (Reference?) and found to be almost the same. However, it is known that the latter compound has a tetragonal coordination at the Zn centre and the former has a planar square coordination at the Ni centre, for the cases reported to date, and so the extent of delocalization of the electrons of (I) is larger than that of the latter and they would be expected to have different spectra. Thus, a planar structure of the Ni-dmit complex synthesized using the current method was suspected. In order to clarify these two points, the present crystal structure determination of (I) was performed and the results are reported here. Please check rephrasing. \sch
The Ni-dmit complex anion of (I) (17 atoms) exhibits good planarity and the maximum deviation from the least squares plane is 0.043 (2) Å (atoms S1 and S1a the two terminal atoms of the anion). Thus, the close similarity of the two fluorescence emission spectra remains unexplained, assuming there are no mistakes in the spectroscopic measurements. The geometric parameters of the anion of (I) do not differ considerably from those reported (Mentzafos et al., 1988; Valade et al., 1985), although they agree better with the data reported by Mentzafos et al. (1988; Ni, j = 2).
The four S atoms around Ni adopt a centrosymmetric arrangement with each pair of trans S atoms equivalent (Table 1). In our opinion, the four S atoms should not be regarded as equivalent, even within the range of experimental uncertainty; referring to Fig. 1 and Table 1, the Ni1—S4 and Ni1—S5 bond lengths are 2.1541 (15) and 2.1638 (15) Å, respectively, and the S4—Ni1—S5a and S4—Ni1—S5 bond angles are 87.37 (6) and 92.63 (6)°, respectively. A similar result was seen in the molecular structure of nickel diethyldithiocarbamate (Bonamico et al., 1965). As far as the tetra-n-butylammonium cation is concerned (Fig. 1), two of the four butyl chains are disordered, as observed and described by Mentzafos et al. (1988).
The crystal packing of (I) is basically isostructural with that of the corresponding Pt complex (Mentzafos et al., 1988), but there are fairly large differences from the structures reported (Table 2) for other compounds of the same chemical composition (Mentzafos et al., 1988, and references therein). Taking only the packing of the Ni complex anion into account, and referring to Fig. 2, the anions form stacks along the c axis. In the stack, the anions form a zigzag array and there are short S···S contacts [3.597 (2) Å for both S4···S4 and S4a···S4a] between neighbouring anions, but there are no short interstack S···S contacts. All of these results are in almost perfect agreement with those of the corresponding Pt complex (Mentzafos et al., 1988).