Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807006149/is2132sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536807006149/is2132Isup2.hkl |
CCDC reference: 640397
Data collection: SMART (Bruker, 2000); cell refinement: SAINT (Bruker, 2000); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Bruker, 2000); software used to prepare material for publication: SHELXTL.
[Ni(C6H4N2O4S)(H2O)3]·2.5H2O | F(000) = 1480 |
Mr = 357.97 | Dx = 1.820 Mg m−3 |
Orthorhombic, Pbcn | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2n 2ab | Cell parameters from 996 reflections |
a = 25.272 (5) Å | θ = 4.3–27.6° |
b = 7.5122 (16) Å | µ = 1.69 mm−1 |
c = 13.764 (3) Å | T = 293 K |
V = 2613.1 (9) Å3 | Block, green |
Z = 8 | 0.28 × 0.25 × 0.20 mm |
Bruker SMART APEX CCD area-detector diffractometer | 2557 independent reflections |
Radiation source: fine-focus sealed tube | 2222 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.089 |
φ and ω scans | θmax = 26.0°, θmin = 2.8° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −30→30 |
Tmin = 0.62, Tmax = 0.71 | k = −6→9 |
12876 measured reflections | l = −16→16 |
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)] = 0.038 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.111 | H-atom parameters constrained |
S = 1.00 | w = 1/[σ2(Fo2) + (0.0712P)2 + 1.4863P] where P = (Fo2 + 2Fc2)/3 |
2557 reflections | (Δ/σ)max < 0.001 |
177 parameters | Δρmax = 0.55 e Å−3 |
0 restraints | Δρmin = −0.51 e Å−3 |
Experimental. A thermogravimetric analysis gave the loss of all uncoordinated water molecules between 110 and 140 °C (13.2% observed, 12.57% calculated). On further heating, the compound lost weight continuously, corresponding to the preliminary decomposition of the whole framework, and an obvious decomposition was observed at 280 °C, corresponding to the final decomposition of the whole framework. |
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) | |
C1 | 0.19767 (10) | 0.2131 (3) | 0.79562 (19) | 0.0232 (5) | |
C2 | 0.25131 (10) | 0.2292 (4) | 0.80848 (19) | 0.0269 (6) | |
H2 | 0.2645 | 0.2800 | 0.8651 | 0.032* | |
C3 | 0.28603 (11) | 0.1697 (3) | 0.7373 (2) | 0.0240 (6) | |
C4 | 0.21006 (10) | 0.0838 (3) | 0.64389 (18) | 0.0224 (5) | |
C5 | 0.12182 (10) | −0.0726 (3) | 0.5623 (2) | 0.0254 (6) | |
H5A | 0.1092 | −0.1555 | 0.5135 | 0.030* | |
H5B | 0.1222 | −0.1350 | 0.6240 | 0.030* | |
C6 | 0.08260 (11) | 0.0801 (4) | 0.57045 (19) | 0.0262 (6) | |
N1 | 0.17726 (9) | 0.1375 (3) | 0.71028 (16) | 0.0233 (5) | |
N2 | 0.26281 (8) | 0.0965 (3) | 0.65380 (15) | 0.0245 (5) | |
H2A | 0.2848 | 0.0822 | 0.6062 | 0.029* | |
Ni1 | 0.100163 (13) | 0.17208 (4) | 0.76578 (3) | 0.02264 (15) | |
O1 | 0.16111 (7) | 0.2609 (3) | 0.85411 (13) | 0.0286 (4) | |
O2 | 0.33560 (8) | 0.1748 (2) | 0.73959 (15) | 0.0311 (5) | |
O3 | 0.05587 (7) | 0.0872 (3) | 0.64912 (13) | 0.0288 (4) | |
O4 | 0.07691 (10) | 0.1831 (3) | 0.50215 (16) | 0.0472 (6) | |
O5 | 0.10126 (8) | −0.0831 (3) | 0.81986 (14) | 0.0318 (5) | |
H5D | 0.1224 | −0.1460 | 0.7862 | 0.038* | |
H5C | 0.1116 | −0.0816 | 0.8786 | 0.038* | |
O6 | 0.09224 (8) | 0.4218 (3) | 0.70658 (17) | 0.0388 (5) | |
H6B | 0.1012 | 0.4993 | 0.7484 | 0.047* | |
H6A | 0.1121 | 0.4306 | 0.6570 | 0.047* | |
O7 | 0.04217 (7) | 0.2261 (3) | 0.86169 (15) | 0.0334 (5) | |
H7A | 0.0123 | 0.2024 | 0.8363 | 0.040* | |
H7B | 0.0433 | 0.3357 | 0.8769 | 0.040* | |
O8 | 0.17025 (11) | 0.5103 (3) | 1.00349 (17) | 0.0510 (7) | |
H8A | 0.1765 | 0.4252 | 0.9645 | 0.061* | |
H8B | 0.1426 | 0.5654 | 0.9852 | 0.061* | |
H9B | −0.0281 | 0.5552 | 0.9045 | 0.061* | |
H9A | 0.0178 | 0.6295 | 0.9420 | 0.061* | |
O9 | 0.00541 (12) | 0.5571 (4) | 0.9003 (2) | 0.0692 (8) | |
O10 | 0.0000 | 0.7844 (5) | 0.7500 | 0.0524 (9) | |
H10A | 0.0312 | 0.8088 | 0.7311 | 0.063* | 0.50 |
H10B | −0.0155 | 0.8794 | 0.7676 | 0.063* | 0.50 |
S1 | 0.18896 (3) | −0.01007 (10) | 0.53348 (5) | 0.0290 (2) |
U11 | U22 | U33 | U12 | U13 | U23 | |
C1 | 0.0283 (14) | 0.0219 (12) | 0.0193 (12) | −0.0017 (10) | −0.0013 (10) | 0.0016 (10) |
C2 | 0.0284 (13) | 0.0274 (14) | 0.0251 (13) | −0.0006 (11) | −0.0040 (11) | −0.0036 (11) |
C3 | 0.0240 (15) | 0.0191 (14) | 0.0290 (15) | −0.0027 (10) | −0.0013 (10) | 0.0030 (10) |
C4 | 0.0253 (13) | 0.0220 (13) | 0.0200 (12) | −0.0012 (10) | 0.0000 (10) | 0.0030 (10) |
C5 | 0.0251 (13) | 0.0259 (14) | 0.0252 (13) | −0.0005 (11) | 0.0004 (10) | −0.0020 (11) |
C6 | 0.0277 (14) | 0.0293 (14) | 0.0215 (13) | −0.0013 (11) | −0.0018 (11) | −0.0017 (11) |
N1 | 0.0229 (11) | 0.0257 (11) | 0.0212 (11) | −0.0015 (9) | −0.0008 (9) | −0.0017 (9) |
N2 | 0.0226 (11) | 0.0285 (12) | 0.0224 (11) | −0.0012 (9) | 0.0032 (8) | −0.0010 (9) |
Ni1 | 0.0213 (2) | 0.0260 (2) | 0.0207 (2) | −0.00033 (12) | 0.00101 (12) | −0.00109 (13) |
O1 | 0.0263 (9) | 0.0368 (11) | 0.0226 (9) | 0.0016 (8) | 0.0010 (7) | −0.0076 (8) |
O2 | 0.0241 (11) | 0.0294 (11) | 0.0398 (12) | −0.0018 (8) | −0.0007 (8) | −0.0035 (8) |
O3 | 0.0248 (9) | 0.0385 (11) | 0.0231 (10) | 0.0002 (8) | −0.0004 (7) | −0.0035 (8) |
O4 | 0.0655 (16) | 0.0465 (14) | 0.0297 (12) | 0.0239 (12) | 0.0088 (11) | 0.0101 (10) |
O5 | 0.0414 (12) | 0.0314 (11) | 0.0227 (10) | 0.0072 (8) | 0.0048 (8) | 0.0017 (9) |
O6 | 0.0402 (12) | 0.0298 (11) | 0.0464 (13) | −0.0066 (9) | −0.0068 (9) | 0.0047 (10) |
O7 | 0.0256 (10) | 0.0365 (11) | 0.0381 (11) | −0.0019 (8) | 0.0058 (8) | −0.0084 (9) |
O8 | 0.0648 (16) | 0.0505 (15) | 0.0377 (13) | 0.0167 (12) | −0.0196 (11) | −0.0114 (11) |
O9 | 0.092 (2) | 0.0450 (15) | 0.0703 (19) | −0.0004 (14) | 0.0144 (16) | −0.0092 (14) |
O10 | 0.040 (2) | 0.0419 (19) | 0.075 (2) | 0.000 | −0.0025 (16) | 0.000 |
S1 | 0.0279 (4) | 0.0392 (4) | 0.0200 (3) | −0.0010 (3) | 0.0017 (2) | −0.0057 (3) |
C1—O1 | 1.277 (3) | Ni1—O7 | 2.0136 (19) |
C1—C2 | 1.373 (4) | Ni1—O6 | 2.055 (2) |
C1—N1 | 1.403 (3) | Ni1—O5 | 2.057 (2) |
C2—C3 | 1.389 (4) | Ni1—O3 | 2.0585 (19) |
C2—H2 | 0.93 | Ni1—O1 | 2.0725 (19) |
C3—O2 | 1.254 (4) | O5—H5D | 0.85 |
C3—N2 | 1.403 (3) | O5—H5C | 0.85 |
C4—N1 | 1.298 (3) | O6—H6B | 0.85 |
C4—N2 | 1.344 (3) | O6—H6A | 0.85 |
C4—S1 | 1.758 (3) | O7—H7A | 0.85 |
C5—C6 | 1.520 (4) | O7—H7B | 0.85 |
C5—S1 | 1.805 (3) | O8—H8A | 0.85 |
C5—H5A | 0.97 | O8—H8B | 0.85 |
C5—H5B | 0.97 | O9—H9B | 0.85 |
C6—O4 | 1.226 (3) | O9—H9A | 0.85 |
C6—O3 | 1.277 (3) | O10—H10A | 0.85 |
N1—Ni1 | 2.109 (2) | O10—H10B | 0.85 |
N2—H2A | 0.87 | ||
O1—C1—C2 | 127.5 (2) | O6—Ni1—O5 | 174.68 (8) |
O1—C1—N1 | 112.1 (2) | O7—Ni1—O3 | 100.25 (8) |
C2—C1—N1 | 120.4 (2) | O6—Ni1—O3 | 85.45 (8) |
C1—C2—C3 | 120.3 (2) | O5—Ni1—O3 | 90.05 (8) |
C1—C2—H2 | 119.9 | O7—Ni1—O1 | 95.26 (8) |
C3—C2—H2 | 119.8 | O6—Ni1—O1 | 90.64 (8) |
O2—C3—C2 | 127.1 (3) | O5—Ni1—O1 | 94.45 (8) |
O2—C3—N2 | 116.8 (2) | O3—Ni1—O1 | 164.01 (7) |
C2—C3—N2 | 116.1 (2) | O7—Ni1—N1 | 159.18 (8) |
N1—C4—N2 | 122.7 (2) | O6—Ni1—N1 | 93.37 (9) |
N1—C4—S1 | 122.6 (2) | O5—Ni1—N1 | 90.22 (8) |
N2—C4—S1 | 114.65 (19) | O3—Ni1—N1 | 100.47 (8) |
C6—C5—S1 | 115.65 (19) | O1—Ni1—N1 | 64.24 (8) |
C6—C5—H5A | 108.8 | C1—O1—Ni1 | 94.45 (15) |
S1—C5—H5A | 108.8 | C6—O3—Ni1 | 112.75 (16) |
C6—C5—H5B | 107.9 | Ni1—O5—H5D | 109.2 |
S1—C5—H5B | 108.0 | Ni1—O5—H5C | 109.6 |
H5A—C5—H5B | 107.4 | H5D—O5—H5C | 109.5 |
O4—C6—O3 | 124.2 (3) | Ni1—O6—H6B | 109.3 |
O4—C6—C5 | 119.8 (2) | Ni1—O6—H6A | 109.4 |
O3—C6—C5 | 116.0 (2) | H6B—O6—H6A | 109.5 |
C4—N1—C1 | 118.7 (2) | Ni1—O7—H7A | 109.5 |
C4—N1—Ni1 | 152.05 (19) | Ni1—O7—H7B | 109.4 |
C1—N1—Ni1 | 89.22 (15) | H7A—O7—H7B | 109.5 |
C4—N2—C3 | 121.7 (2) | H8A—O8—H8B | 109.5 |
C4—N2—H2A | 123.4 | H9B—O9—H9A | 109.4 |
C3—N2—H2A | 113.6 | H10A—O10—H10B | 109.5 |
O7—Ni1—O6 | 90.30 (9) | C4—S1—C5 | 101.50 (12) |
O7—Ni1—O5 | 87.73 (8) |
D—H···A | D—H | H···A | D···A | D—H···A |
O10—H10B···O5i | 0.85 | 2.50 | 2.909 (2) | 111 |
O10—H10B···O3i | 0.85 | 2.19 | 3.016 (3) | 165 |
O10—H10A···O3ii | 0.85 | 2.46 | 3.016 (3) | 124 |
O10—H10A···O5ii | 0.85 | 2.30 | 2.909 (2) | 129 |
O8—H8B···O4iii | 0.85 | 2.53 | 3.297 (4) | 151 |
O8—H8A···O1 | 0.85 | 2.00 | 2.791 (3) | 156 |
O7—H7A···O3iv | 0.85 | 1.94 | 2.693 (3) | 147 |
O6—H6B···O2v | 0.85 | 2.07 | 2.673 (3) | 127 |
O5—H5C···O4vi | 0.85 | 2.06 | 2.690 (3) | 131 |
O5—H5D···O2vii | 0.85 | 1.83 | 2.660 (3) | 165 |
N2—H2A···O8viii | 0.87 | 1.94 | 2.790 (3) | 166 |
Symmetry codes: (i) −x, y+1, −z+3/2; (ii) x, y+1, z; (iii) x, −y+1, z+1/2; (iv) −x, y, −z+3/2; (v) −x+1/2, y+1/2, z; (vi) x, −y, z+1/2; (vii) −x+1/2, y−1/2, z; (viii) −x+1/2, −y+1/2, z−1/2. |