Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536804004854/wk6011sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536804004854/wk6011Isup2.hkl |
CCDC reference: 238632
Data collection: CrysAlis CCD (Oxford Diffraction, 2003); cell refinement: CrysAlis RED (Oxford Diffraction, 2003); data reduction: CrysAlis RED; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 (Farrugia, 1997); software used to prepare material for publication: WinGX (Farrugia, 1999) and PARST97 (Nardelli, 1995).
[Ni(C10H9O2)2(C2H6OS)2] | F(000) = 564 |
Mr = 537.31 | Dx = 1.489 Mg m−3 |
Monoclinic, P21/a | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2yab | Cell parameters from 5096 reflections |
a = 7.3772 (17) Å | θ = 2.1–21.3° |
b = 13.453 (2) Å | µ = 1.02 mm−1 |
c = 12.085 (2) Å | T = 100 K |
β = 92.026 (18)° | Block, green |
V = 1198.7 (4) Å3 | 0.30 × 0.14 × 0.10 mm |
Z = 2 |
Oxford Diffraction Xcalibur CCD diffractometer | 3516 independent reflections |
Radiation source: fine-focus sealed tube | 2561 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.060 |
ω scans | θmax = 30.1°, θmin = 4.1° |
Absorption correction: analytical (Alcock, 1970) | h = −10→10 |
Tmin = 0.818, Tmax = 0.912 | k = −18→18 |
32533 measured reflections | l = −17→17 |
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)] = 0.035 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.064 | H-atom parameters constrained |
S = 0.95 | w = 1/[σ2(Fo2) + (0.0219P)2] where P = (Fo2 + 2Fc2)/3 |
3516 reflections | (Δ/σ)max < 0.001 |
154 parameters | Δρmax = 0.57 e Å−3 |
0 restraints | Δρmin = −0.32 e Å−3 |
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. |
x | y | z | Uiso*/Ueq | ||
Ni | −0.5000 | 0.0000 | 0.5000 | 0.01175 (9) | |
O12 | −0.57523 (16) | −0.12538 (9) | 0.57711 (10) | 0.0143 (3) | |
O11 | −0.42381 (16) | 0.05995 (9) | 0.64556 (10) | 0.0142 (3) | |
O2 | −0.23567 (17) | −0.05838 (9) | 0.49094 (10) | 0.0156 (3) | |
S2 | −0.16864 (6) | −0.11127 (4) | 0.38974 (4) | 0.01535 (11) | |
C21 | −0.0646 (3) | −0.01827 (14) | 0.30905 (16) | 0.0213 (5) | |
H21B | 0.0288 | 0.0143 | 0.3529 | 0.032* | |
H21A | −0.1540 | 0.0296 | 0.2850 | 0.032* | |
H21C | −0.0123 | −0.0485 | 0.2457 | 0.032* | |
C22 | 0.0312 (2) | −0.17378 (14) | 0.43539 (16) | 0.0183 (4) | |
H22C | −0.0001 | −0.2295 | 0.4804 | 0.028* | |
H22B | 0.1071 | −0.1290 | 0.4781 | 0.028* | |
H22A | 0.0952 | −0.1967 | 0.3725 | 0.028* | |
C11 | −0.6024 (3) | −0.24838 (14) | 0.71412 (16) | 0.0199 (4) | |
H11A | −0.6916 | −0.2751 | 0.6626 | 0.030* | |
H11C | −0.6515 | −0.2457 | 0.7866 | 0.030* | |
H11B | −0.4967 | −0.2901 | 0.7159 | 0.030* | |
C12 | −0.5510 (2) | −0.14487 (14) | 0.67841 (16) | 0.0150 (4) | |
C13 | −0.4801 (2) | −0.07943 (14) | 0.75847 (15) | 0.0159 (4) | |
H13 | −0.4732 | −0.1019 | 0.8313 | 0.019* | |
C14 | −0.4186 (2) | 0.01675 (14) | 0.73870 (14) | 0.0132 (4) | |
C15 | −0.3386 (2) | 0.07743 (15) | 0.83229 (15) | 0.0150 (4) | |
C16 | −0.2716 (3) | 0.03618 (17) | 0.93050 (16) | 0.0263 (5) | |
H16 | −0.2812 | −0.0319 | 0.9423 | 0.032* | |
C17 | −0.1906 (3) | 0.09593 (19) | 1.01094 (17) | 0.0333 (6) | |
H17 | −0.1454 | 0.0677 | 1.0765 | 0.040* | |
C18 | −0.1761 (3) | 0.19714 (18) | 0.99491 (17) | 0.0293 (5) | |
H18 | −0.1213 | 0.2368 | 1.0495 | 0.035* | |
C19 | −0.2425 (3) | 0.23897 (16) | 0.89860 (17) | 0.0252 (5) | |
H19 | −0.2337 | 0.3072 | 0.8875 | 0.030* | |
C110 | −0.3227 (2) | 0.17923 (15) | 0.81806 (16) | 0.0186 (4) | |
H110 | −0.3671 | 0.2080 | 0.7526 | 0.022* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Ni | 0.01212 (16) | 0.01274 (19) | 0.01040 (17) | −0.00004 (15) | 0.00074 (12) | −0.00066 (15) |
O12 | 0.0155 (6) | 0.0140 (7) | 0.0136 (7) | −0.0005 (5) | 0.0011 (5) | 0.0002 (5) |
O11 | 0.0173 (7) | 0.0133 (7) | 0.0120 (7) | 0.0001 (6) | −0.0001 (5) | 0.0010 (6) |
O2 | 0.0134 (6) | 0.0196 (8) | 0.0140 (7) | 0.0023 (6) | 0.0009 (5) | −0.0039 (6) |
S2 | 0.0122 (2) | 0.0167 (3) | 0.0172 (2) | 0.0000 (2) | 0.00126 (18) | −0.0035 (2) |
C21 | 0.0193 (10) | 0.0251 (13) | 0.0197 (10) | 0.0073 (9) | 0.0041 (8) | 0.0068 (9) |
C22 | 0.0176 (10) | 0.0152 (11) | 0.0225 (11) | 0.0041 (8) | 0.0039 (8) | 0.0031 (9) |
C11 | 0.0205 (10) | 0.0186 (11) | 0.0206 (11) | −0.0015 (9) | 0.0003 (8) | 0.0033 (9) |
C12 | 0.0099 (8) | 0.0157 (11) | 0.0196 (10) | 0.0033 (8) | 0.0032 (7) | 0.0027 (8) |
C13 | 0.0171 (9) | 0.0174 (11) | 0.0131 (10) | 0.0013 (8) | 0.0005 (7) | 0.0032 (8) |
C14 | 0.0084 (8) | 0.0190 (12) | 0.0124 (9) | 0.0042 (8) | 0.0013 (7) | −0.0014 (8) |
C15 | 0.0118 (9) | 0.0205 (11) | 0.0129 (9) | −0.0002 (8) | 0.0023 (7) | −0.0029 (8) |
C16 | 0.0306 (12) | 0.0291 (13) | 0.0189 (11) | −0.0059 (10) | −0.0035 (9) | 0.0031 (9) |
C17 | 0.0363 (13) | 0.0505 (17) | 0.0125 (11) | −0.0073 (12) | −0.0068 (9) | 0.0033 (10) |
C18 | 0.0249 (11) | 0.0438 (16) | 0.0193 (11) | −0.0100 (11) | 0.0016 (9) | −0.0132 (10) |
C19 | 0.0231 (11) | 0.0255 (13) | 0.0272 (12) | −0.0041 (9) | 0.0031 (9) | −0.0093 (10) |
C110 | 0.0163 (9) | 0.0229 (12) | 0.0165 (10) | 0.0010 (9) | −0.0003 (8) | −0.0032 (9) |
Ni—O11 | 1.9978 (12) | C11—H11B | 0.9600 |
Ni—O12 | 2.0145 (13) | C12—C13 | 1.396 (3) |
Ni—O2 | 2.1087 (13) | C13—C14 | 1.394 (2) |
O12—C12 | 1.259 (2) | C13—H13 | 0.9300 |
O11—C14 | 1.266 (2) | C14—C15 | 1.499 (2) |
O2—S2 | 1.5131 (13) | C15—C16 | 1.385 (3) |
S2—C22 | 1.7688 (18) | C15—C110 | 1.386 (3) |
S2—C21 | 1.7772 (19) | C16—C17 | 1.381 (3) |
C21—H21B | 0.9600 | C16—H16 | 0.9300 |
C21—H21A | 0.9600 | C17—C18 | 1.380 (3) |
C21—H21C | 0.9600 | C17—H17 | 0.9300 |
C22—H22C | 0.9600 | C18—C19 | 1.368 (3) |
C22—H22B | 0.9600 | C18—H18 | 0.9300 |
C22—H22A | 0.9600 | C19—C110 | 1.379 (3) |
C11—C12 | 1.510 (3) | C19—H19 | 0.9300 |
C11—H11A | 0.9600 | C110—H110 | 0.9300 |
C11—H11C | 0.9600 | ||
O11—Ni—O12 | 90.24 (5) | O12—C12—C13 | 125.43 (18) |
O11—Ni—O2 | 87.95 (5) | O12—C12—C11 | 116.20 (17) |
O12—Ni—O2 | 89.00 (5) | C13—C12—C11 | 118.37 (17) |
C12—O12—Ni | 126.33 (12) | C14—C13—C12 | 125.63 (17) |
C14—O11—Ni | 126.60 (12) | C14—C13—H13 | 117.2 |
S2—O2—Ni | 123.12 (7) | C12—C13—H13 | 117.2 |
O2—S2—C22 | 105.31 (8) | O11—C14—C13 | 125.34 (16) |
O2—S2—C21 | 105.80 (9) | O11—C14—C15 | 114.80 (16) |
C22—S2—C21 | 97.72 (9) | C13—C14—C15 | 119.86 (16) |
S2—C21—H21B | 109.5 | C16—C15—C110 | 118.23 (18) |
S2—C21—H21A | 109.5 | C16—C15—C14 | 123.18 (18) |
H21B—C21—H21A | 109.5 | C110—C15—C14 | 118.52 (16) |
S2—C21—H21C | 109.5 | C17—C16—C15 | 120.1 (2) |
H21B—C21—H21C | 109.5 | C17—C16—H16 | 119.9 |
H21A—C21—H21C | 109.5 | C15—C16—H16 | 119.9 |
S2—C22—H22C | 109.5 | C18—C17—C16 | 120.6 (2) |
S2—C22—H22B | 109.5 | C18—C17—H17 | 119.7 |
H22C—C22—H22B | 109.5 | C16—C17—H17 | 119.7 |
S2—C22—H22A | 109.5 | C19—C18—C17 | 119.9 (2) |
H22C—C22—H22A | 109.5 | C19—C18—H18 | 120.1 |
H22B—C22—H22A | 109.5 | C17—C18—H18 | 120.1 |
C12—C11—H11A | 109.5 | C18—C19—C110 | 119.5 (2) |
C12—C11—H11C | 109.5 | C18—C19—H19 | 120.2 |
H11A—C11—H11C | 109.5 | C110—C19—H19 | 120.2 |
C12—C11—H11B | 109.5 | C19—C110—C15 | 121.63 (19) |
H11A—C11—H11B | 109.5 | C19—C110—H110 | 119.2 |
H11C—C11—H11B | 109.5 | C15—C110—H110 | 119.2 |