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The title ionic compound, [Ni(C
12H
12N
2)(H
2O)
4]SO
4·H
2O, is composed of an Ni
II cation coordinated by a chelating 4,4'-dimethyl-2,2'-bipyridine ligand
via its two N atoms [mean Ni-N = 2.056 (2) Å] and by four aqua ligands [mean Ni-O = 2.073 (9) Å], the net charge being balanced by an external sulfate anion. The whole structure is stabilized by a solvent water molecule. Even though the individual constituents are rather featureless, they generate an extremely complex supramolecular structure consisting of a central hydrogen-bonded two-dimensional hydrophilic nucleus made up of complex cations, sulfate anions and coordinated and solvent water molecules, with pendant hydrophobic 4,4'-dimethyl-2,2'-bipyridine ligands which interact laterally with their neighbours
via -
interactions. The structure is compared with closely related analogues in the literature.
Supporting information
CCDC reference: 934598
Data collection: CrysAlis PRO (Oxford Diffraction, 2009); cell refinement: CrysAlis PRO (Oxford Diffraction, 2009); data reduction: CrysAlis PRO (Oxford Diffraction, 2009); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXL97 (Sheldrick, 2008), RPLUTO (CCDC, 2007) and PLATON
(Spek, 2009).
Tetraaqua(4,4'-dimethyl-2,2'-bipyridine-
κ2N,
N')nickel(II)
sulfate monohydrate
top
Crystal data top
[Ni(C12H12N2)(H2O)4]SO4·H2O | F(000) = 896 |
Mr = 429.09 | Dx = 1.642 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2yn | Cell parameters from 3870 reflections |
a = 11.8007 (3) Å | θ = 2.7–25.2° |
b = 11.7095 (3) Å | µ = 1.29 mm−1 |
c = 13.6967 (3) Å | T = 150 K |
β = 113.530 (12)° | Prism, light blue |
V = 1735.24 (17) Å3 | 0.48 × 0.18 × 0.14 mm |
Z = 4 | |
Data collection top
Oxford Gemini CCD S Ultra diffractometer | 3599 reflections with I > 2σ(I) |
ω scans, thick slices | Rint = 0.014 |
Absorption correction: multi-scan (CrysAlis PRO; Oxford Diffraction, 2009) | θmax = 27.8°, θmin = 1.9° |
Tmin = 0.76, Tmax = 0.84 | h = −15→15 |
14064 measured reflections | k = −15→14 |
3811 independent reflections | l = −17→17 |
Refinement top
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)] = 0.027 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.075 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.07 | w = 1/[σ2(Fo2) + (0.0462P)2 + 0.8214P] where P = (Fo2 + 2Fc2)/3 |
3811 reflections | (Δ/σ)max = 0.008 |
258 parameters | Δρmax = 0.54 e Å−3 |
15 restraints | Δρmin = −0.49 e Å−3 |
Special details top
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. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | Occ. (<1) |
Ni1 | 0.881378 (16) | 0.496228 (14) | 0.221537 (14) | 0.01282 (8) | |
N1 | 0.99139 (11) | 0.59788 (11) | 0.17338 (10) | 0.0155 (2) | |
N2 | 0.97379 (11) | 0.37435 (11) | 0.17329 (9) | 0.0143 (2) | |
C1 | 0.99794 (15) | 0.71205 (13) | 0.17923 (12) | 0.0191 (3) | |
H1 | 0.9413 | 0.7519 | 0.2003 | 0.023* | |
C2 | 1.08334 (15) | 0.77449 (13) | 0.15595 (13) | 0.0212 (3) | |
H2 | 1.0854 | 0.8554 | 0.1621 | 0.025* | |
C3 | 1.16645 (14) | 0.71816 (13) | 0.12344 (12) | 0.0197 (3) | |
C4 | 1.15978 (14) | 0.59903 (13) | 0.11793 (12) | 0.0185 (3) | |
H4 | 1.2151 | 0.5573 | 0.0966 | 0.022* | |
C5 | 1.07257 (13) | 0.54165 (13) | 0.14363 (11) | 0.0159 (3) | |
C6 | 1.06101 (13) | 0.41472 (13) | 0.14155 (11) | 0.0151 (3) | |
C7 | 1.13319 (14) | 0.34198 (13) | 0.10983 (12) | 0.0180 (3) | |
H7 | 1.1941 | 0.3725 | 0.0882 | 0.022* | |
C8 | 1.11601 (14) | 0.22372 (13) | 0.10986 (12) | 0.0187 (3) | |
C9 | 1.02545 (15) | 0.18412 (13) | 0.14215 (12) | 0.0200 (3) | |
H9 | 1.0105 | 0.1045 | 0.1432 | 0.024* | |
C10 | 0.95702 (14) | 0.26143 (13) | 0.17279 (12) | 0.0176 (3) | |
H10 | 0.8953 | 0.2329 | 0.1945 | 0.021* | |
C11 | 1.25956 (16) | 0.78285 (14) | 0.09601 (14) | 0.0250 (3) | |
H11A | 1.3185 | 0.7291 | 0.0872 | 0.037* | 0.50 |
H11B | 1.3039 | 0.8366 | 0.1534 | 0.037* | 0.50 |
H11C | 1.2171 | 0.8250 | 0.0295 | 0.037* | 0.50 |
H11D | 1.2412 | 0.8647 | 0.0929 | 0.037* | 0.50 |
H11E | 1.2558 | 0.7572 | 0.0267 | 0.037* | 0.50 |
H11F | 1.3426 | 0.7689 | 0.1506 | 0.037* | 0.50 |
C12 | 1.19356 (16) | 0.14301 (14) | 0.07717 (14) | 0.0260 (3) | |
H12A | 1.2466 | 0.1868 | 0.0511 | 0.039* | 0.50 |
H12B | 1.1396 | 0.0927 | 0.0205 | 0.039* | 0.50 |
H12C | 1.2451 | 0.0969 | 0.1386 | 0.039* | 0.50 |
H12D | 1.1742 | 0.0642 | 0.0890 | 0.039* | 0.50 |
H12E | 1.2813 | 0.1582 | 0.1196 | 0.039* | 0.50 |
H12F | 1.1758 | 0.1540 | 0.0015 | 0.039* | 0.50 |
S1 | 0.46711 (3) | 0.28090 (3) | −0.00349 (3) | 0.01434 (10) | |
O1 | 0.44429 (10) | 0.33060 (9) | −0.10842 (8) | 0.0192 (2) | |
O2 | 0.59885 (10) | 0.28740 (9) | 0.06801 (8) | 0.0191 (2) | |
O3 | 0.39200 (10) | 0.34164 (9) | 0.04476 (8) | 0.0193 (2) | |
O4 | 0.42903 (10) | 0.15839 (9) | −0.01878 (8) | 0.0183 (2) | |
O1W | 1.02352 (11) | 0.49105 (9) | 0.37309 (9) | 0.0167 (2) | |
H1WA | 1.0124 (17) | 0.4397 (10) | 0.4106 (12) | 0.020* | |
H1WB | 1.0407 (17) | 0.5513 (9) | 0.4098 (12) | 0.020* | |
O2W | 0.73828 (10) | 0.48140 (9) | 0.07310 (9) | 0.0165 (2) | |
H2WA | 0.6904 (13) | 0.4267 (10) | 0.0664 (14) | 0.020* | |
H2WB | 0.6956 (14) | 0.5380 (10) | 0.0415 (14) | 0.020* | |
O3W | 0.77982 (9) | 0.38622 (9) | 0.27347 (8) | 0.0163 (2) | |
H3WA | 0.7084 (10) | 0.4105 (15) | 0.2607 (12) | 0.020* | |
H3WB | 0.8139 (13) | 0.3730 (15) | 0.3392 (8) | 0.020* | |
O4W | 0.79553 (10) | 0.63138 (9) | 0.26225 (9) | 0.0197 (2) | |
H4WA | 0.7307 (12) | 0.6573 (14) | 0.2157 (10) | 0.024* | |
H4WB | 0.8260 (15) | 0.6806 (13) | 0.3111 (10) | 0.024* | |
O5W | 0.54228 (11) | 0.46991 (10) | 0.22121 (9) | 0.0217 (2) | |
H5WA | 0.5423 (17) | 0.5323 (9) | 0.1903 (13) | 0.026* | |
H5WB | 0.4957 (15) | 0.4261 (11) | 0.1729 (11) | 0.026* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Ni1 | 0.01226 (12) | 0.01313 (12) | 0.01317 (12) | 0.00039 (6) | 0.00518 (9) | −0.00047 (6) |
N1 | 0.0149 (6) | 0.0167 (6) | 0.0149 (6) | −0.0005 (5) | 0.0060 (5) | 0.0010 (5) |
N2 | 0.0129 (6) | 0.0166 (6) | 0.0124 (5) | 0.0015 (5) | 0.0038 (4) | −0.0006 (5) |
C1 | 0.0204 (7) | 0.0171 (7) | 0.0209 (7) | 0.0007 (6) | 0.0093 (6) | −0.0004 (6) |
C2 | 0.0250 (8) | 0.0159 (7) | 0.0229 (8) | −0.0025 (6) | 0.0097 (6) | −0.0002 (6) |
C3 | 0.0200 (7) | 0.0233 (8) | 0.0148 (7) | −0.0048 (6) | 0.0059 (6) | −0.0009 (6) |
C4 | 0.0167 (7) | 0.0220 (7) | 0.0181 (7) | −0.0016 (6) | 0.0083 (6) | −0.0020 (6) |
C5 | 0.0156 (7) | 0.0181 (7) | 0.0125 (6) | −0.0001 (6) | 0.0039 (5) | −0.0014 (5) |
C6 | 0.0137 (6) | 0.0175 (7) | 0.0129 (6) | 0.0001 (5) | 0.0041 (5) | 0.0006 (5) |
C7 | 0.0161 (7) | 0.0205 (7) | 0.0183 (7) | −0.0002 (6) | 0.0079 (6) | −0.0004 (6) |
C8 | 0.0189 (7) | 0.0200 (8) | 0.0174 (7) | 0.0040 (6) | 0.0074 (6) | −0.0007 (6) |
C9 | 0.0240 (8) | 0.0151 (7) | 0.0212 (7) | 0.0009 (6) | 0.0094 (6) | 0.0009 (6) |
C10 | 0.0185 (7) | 0.0186 (7) | 0.0167 (7) | −0.0009 (6) | 0.0083 (6) | 0.0003 (6) |
C11 | 0.0250 (8) | 0.0263 (8) | 0.0256 (8) | −0.0085 (6) | 0.0122 (7) | −0.0008 (6) |
C12 | 0.0275 (8) | 0.0225 (8) | 0.0332 (9) | 0.0055 (7) | 0.0177 (7) | −0.0018 (7) |
S1 | 0.01558 (18) | 0.01209 (17) | 0.01343 (18) | 0.00009 (13) | 0.00376 (13) | 0.00039 (12) |
O1 | 0.0211 (5) | 0.0182 (5) | 0.0167 (5) | −0.0003 (4) | 0.0058 (4) | 0.0031 (4) |
O2 | 0.0156 (5) | 0.0190 (5) | 0.0190 (5) | 0.0003 (4) | 0.0030 (4) | 0.0006 (4) |
O3 | 0.0193 (5) | 0.0180 (5) | 0.0207 (5) | 0.0022 (4) | 0.0081 (4) | −0.0003 (4) |
O4 | 0.0227 (5) | 0.0128 (5) | 0.0166 (5) | −0.0018 (4) | 0.0050 (4) | −0.0004 (4) |
O1W | 0.0182 (6) | 0.0157 (5) | 0.0148 (5) | −0.0010 (4) | 0.0052 (4) | −0.0014 (4) |
O2W | 0.0146 (5) | 0.0160 (5) | 0.0165 (5) | 0.0009 (4) | 0.0037 (4) | 0.0015 (4) |
O3W | 0.0141 (5) | 0.0184 (5) | 0.0149 (5) | 0.0003 (4) | 0.0042 (4) | 0.0019 (4) |
O4W | 0.0167 (5) | 0.0178 (5) | 0.0201 (5) | 0.0045 (4) | 0.0027 (4) | −0.0048 (4) |
O5W | 0.0248 (6) | 0.0186 (5) | 0.0203 (5) | −0.0022 (5) | 0.0076 (5) | −0.0011 (4) |
Geometric parameters (Å, º) top
Ni1—N1 | 2.0545 (12) | C11—H11A | 0.9800 |
Ni1—N2 | 2.0587 (12) | C11—H11B | 0.9800 |
Ni1—O2W | 2.0673 (11) | C11—H11C | 0.9800 |
Ni1—O3W | 2.0694 (11) | C11—H11D | 0.9800 |
Ni1—O4W | 2.0719 (11) | C11—H11E | 0.9800 |
Ni1—O1W | 2.0847 (12) | C11—H11F | 0.9800 |
N1—C1 | 1.3397 (19) | C12—H12A | 0.9800 |
N1—C5 | 1.3524 (19) | C12—H12B | 0.9800 |
N2—C10 | 1.3366 (19) | C12—H12C | 0.9800 |
N2—C6 | 1.3524 (18) | C12—H12D | 0.9800 |
C1—C2 | 1.381 (2) | C12—H12E | 0.9800 |
C1—H1 | 0.9500 | C12—H12F | 0.9800 |
C2—C3 | 1.394 (2) | S1—O2 | 1.4717 (11) |
C2—H2 | 0.9500 | S1—O1 | 1.4724 (11) |
C3—C4 | 1.397 (2) | S1—O3 | 1.4819 (11) |
C3—C11 | 1.501 (2) | S1—O4 | 1.4928 (10) |
C4—C5 | 1.387 (2) | O1W—H1WA | 0.834 (9) |
C4—H4 | 0.9500 | O1W—H1WB | 0.842 (9) |
C5—C6 | 1.492 (2) | O2W—H2WA | 0.834 (9) |
C6—C7 | 1.391 (2) | O2W—H2WB | 0.841 (9) |
C7—C8 | 1.400 (2) | O3W—H3WA | 0.839 (9) |
C7—H7 | 0.9500 | O3W—H3WB | 0.841 (9) |
C8—C9 | 1.389 (2) | O4W—H4WA | 0.833 (9) |
C8—C12 | 1.503 (2) | O4W—H4WB | 0.847 (9) |
C9—C10 | 1.385 (2) | O5W—H5WA | 0.844 (9) |
C9—H9 | 0.9500 | O5W—H5WB | 0.845 (9) |
C10—H10 | 0.9500 | | |
| | | |
N1—Ni1—N2 | 79.34 (5) | H11B—C11—H11C | 109.5 |
N1—Ni1—O2W | 96.07 (5) | C3—C11—H11D | 109.5 |
N2—Ni1—O2W | 87.45 (5) | H11A—C11—H11D | 141.1 |
N1—Ni1—O3W | 176.28 (4) | H11B—C11—H11D | 56.3 |
N2—Ni1—O3W | 97.61 (5) | H11C—C11—H11D | 56.3 |
O2W—Ni1—O3W | 85.87 (4) | C3—C11—H11E | 109.5 |
N1—Ni1—O4W | 94.78 (5) | H11A—C11—H11E | 56.3 |
N2—Ni1—O4W | 173.98 (5) | H11B—C11—H11E | 141.1 |
O2W—Ni1—O4W | 91.93 (4) | H11C—C11—H11E | 56.3 |
O3W—Ni1—O4W | 88.31 (5) | H11D—C11—H11E | 109.5 |
N1—Ni1—O1W | 88.63 (5) | C3—C11—H11F | 109.5 |
N2—Ni1—O1W | 88.89 (4) | H11A—C11—H11F | 56.3 |
O2W—Ni1—O1W | 173.41 (4) | H11B—C11—H11F | 56.3 |
O3W—Ni1—O1W | 89.19 (4) | H11C—C11—H11F | 141.1 |
O4W—Ni1—O1W | 92.28 (4) | H11D—C11—H11F | 109.5 |
C1—N1—C5 | 118.22 (13) | H11E—C11—H11F | 109.5 |
C1—N1—Ni1 | 126.00 (10) | C8—C12—H12A | 109.5 |
C5—N1—Ni1 | 115.41 (10) | C8—C12—H12B | 109.5 |
C10—N2—C6 | 118.31 (13) | H12A—C12—H12B | 109.5 |
C10—N2—Ni1 | 126.23 (10) | C8—C12—H12C | 109.5 |
C6—N2—Ni1 | 115.44 (10) | H12A—C12—H12C | 109.5 |
N1—C1—C2 | 122.98 (14) | H12B—C12—H12C | 109.5 |
N1—C1—H1 | 118.5 | C8—C12—H12D | 109.5 |
C2—C1—H1 | 118.5 | H12A—C12—H12D | 141.1 |
C1—C2—C3 | 119.62 (14) | H12B—C12—H12D | 56.3 |
C1—C2—H2 | 120.2 | H12C—C12—H12D | 56.3 |
C3—C2—H2 | 120.2 | C8—C12—H12E | 109.5 |
C2—C3—C4 | 117.25 (14) | H12A—C12—H12E | 56.3 |
C2—C3—C11 | 121.33 (14) | H12B—C12—H12E | 141.1 |
C4—C3—C11 | 121.43 (14) | H12C—C12—H12E | 56.3 |
C5—C4—C3 | 120.09 (14) | H12D—C12—H12E | 109.5 |
C5—C4—H4 | 120.0 | C8—C12—H12F | 109.5 |
C3—C4—H4 | 120.0 | H12A—C12—H12F | 56.3 |
N1—C5—C4 | 121.82 (14) | H12B—C12—H12F | 56.3 |
N1—C5—C6 | 114.86 (12) | H12C—C12—H12F | 141.1 |
C4—C5—C6 | 123.32 (13) | H12D—C12—H12F | 109.5 |
N2—C6—C7 | 121.72 (13) | H12E—C12—H12F | 109.5 |
N2—C6—C5 | 114.69 (12) | O2—S1—O1 | 111.23 (6) |
C7—C6—C5 | 123.59 (13) | O2—S1—O3 | 109.84 (6) |
C6—C7—C8 | 119.92 (14) | O1—S1—O3 | 109.68 (6) |
C6—C7—H7 | 120.0 | O2—S1—O4 | 108.78 (6) |
C8—C7—H7 | 120.0 | O1—S1—O4 | 108.38 (6) |
C9—C8—C7 | 117.41 (13) | O3—S1—O4 | 108.88 (6) |
C9—C8—C12 | 121.48 (14) | Ni1—O1W—H1WA | 111.9 (12) |
C7—C8—C12 | 121.11 (14) | Ni1—O1W—H1WB | 118.4 (12) |
C10—C9—C8 | 119.60 (14) | H1WA—O1W—H1WB | 107.1 (13) |
C10—C9—H9 | 120.2 | Ni1—O2W—H2WA | 115.1 (12) |
C8—C9—H9 | 120.2 | Ni1—O2W—H2WB | 121.8 (12) |
N2—C10—C9 | 123.03 (14) | H2WA—O2W—H2WB | 107.9 (13) |
N2—C10—H10 | 118.5 | Ni1—O3W—H3WA | 112.9 (12) |
C9—C10—H10 | 118.5 | Ni1—O3W—H3WB | 112.8 (12) |
C3—C11—H11A | 109.5 | H3WA—O3W—H3WB | 107.3 (12) |
C3—C11—H11B | 109.5 | Ni1—O4W—H4WA | 118.1 (12) |
H11A—C11—H11B | 109.5 | Ni1—O4W—H4WB | 129.3 (12) |
C3—C11—H11C | 109.5 | H4WA—O4W—H4WB | 109.1 (13) |
H11A—C11—H11C | 109.5 | H5WA—O5W—H5WB | 105.3 (13) |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O1W—H1WA···O4i | 0.83 (1) | 2.00 (1) | 2.7959 (15) | 160 (2) |
O1W—H1WB···O4ii | 0.84 (1) | 1.87 (1) | 2.6913 (15) | 164 (2) |
O2W—H2WA···O2 | 0.83 (1) | 1.96 (1) | 2.7895 (15) | 171 (2) |
O2W—H2WB···O3iii | 0.84 (1) | 1.86 (1) | 2.6985 (15) | 172 (2) |
O3W—H3WA···O5W | 0.84 (1) | 1.94 (1) | 2.7800 (16) | 176 (2) |
O3W—H3WB···O4i | 0.84 (1) | 1.91 (1) | 2.7329 (14) | 165 (2) |
O4W—H4WA···O1iii | 0.83 (1) | 2.01 (1) | 2.8082 (15) | 162 (2) |
O4W—H4WB···O2ii | 0.85 (1) | 1.98 (1) | 2.8253 (15) | 176 (2) |
O5W—H5WA···O1iii | 0.84 (1) | 2.00 (1) | 2.8397 (16) | 172 (2) |
O5W—H5WB···O3 | 0.85 (1) | 1.96 (1) | 2.7963 (15) | 171 (2) |
C11—H11E···O2iv | 0.98 | 2.58 | 3.393 (2) | 140 |
C12—H12A···O3v | 0.98 | 2.52 | 3.453 (2) | 158 |
Symmetry codes: (i) x+1/2, −y+1/2, z+1/2; (ii) −x+3/2, y+1/2, −z+1/2; (iii) −x+1, −y+1, −z; (iv) −x+2, −y+1, −z; (v) x+1, y, z. |
Compararison of reported compounds with the general formula
Tr(Lx)(H2O)4.nH2O (Tr is a transition metal) topLigand codes: L1 is 2,2'-bipyridine; L2 is
5,5'-dimethyl-2,2'-bipyridine; L3 is 4,4'-dimethyl-2,2'-bipyridine;
L4 is 1,10-phenanthroline; L5 is 1,10-phenanthroline-5,6-dione;
L6 is 1H-imidazo[4,5-f][1,10]phenanthroline. |
Compound | Tr | Lx | n | Space group | Z | a (Å) | b (Å) | c (Å) | α (°) | β (°) | γ (°) | V (Å3) |
(Ia) | Ni | L1 | 0 | Pbca | 8 | 12.3035 (7) | 11.6560 (7) | 20.7112 (10) | 90 | 90 | 90 | 2970.2 (3) |
(Ib) | Cd | L1 | 0 | P21/c | 4 | 10.262 (2) | 12.073 (2) | 12.357 (3) | 90 | 92.47 (3) | 90 | 1529.5 (10) |
(Ic) | Zn | L2 | 0 | P21/c | 4 | 9.565 (2) | 9.605 (2) | 18.477 (3) | 90 | 102.45 (9) | 90 | 1657.5 (14) |
| | | | | | | | | | | | |
(IIa) | Ni | L3 | 1 | P21/n | 4 | 11.8007 (3) | 11.7095 (3) | 13.6967 (3) | 90 | 113.531 (12) | 90 | 1735.24 (17) |
| | | | | | | | | | | | |
(IIIa) | Zn | L4 | 2 | Pbca | 8 | 8.906 (1) | 18.295 (2) | 21.855 (3) | 90 | 90 | 90 | 3560.9 (15) |
(IIIb) | Mn | L4 | 2 | Pbca | 8 | 8.877 (1) | 18.508 (3) | 22.098 (3) | 90 | 90 | 90 | 3630.602 (14) |
(IIIc) | Cd | L4 | 2 | Pbca | 8 | 8.8398 (9) | 18.700 (2) | 22.349 (2) | 90 | 90 | 90 | 3694.3 (11) |
(IIId) | Co | L4 | 2 | Pbca | 8 | 8.856 (1) | 18.318 (3) | 21.918 (5) | 90 | 90 | 90 | 3555.6 (17) |
(IIIe) | Mn | L5 | 2 | C2/m | 4 | 9.6237 (4) | 13.9117 (6) | 13.8744 (6) | 90 | 97.32 (2) | 90 | 1842.4 (2) |
(IIIf) | Ni | L1 | 2 | P1 | 2 | 7.793 (3) | 9.351 (3) | 11.476 (4) | 87.40 (2) | 96.50 (2) | 102.37 (2) | 811.4 (19) |
(IIIg) | Ni | L6 | 2 | P1 | 2 | 7.266 (2) | 11.112 (3) | 12.913 (4) | 75.676 (4) | 77.393 (5) | 71.423 (5) | 946.4 (15) |
Supplementary Table S4. Hydrogen-bonded chains in (IIa), involving up to
three different primary hydrogen bonds between groups of atoms Gri topThe interactions have the form of Gr1···Gr2···Gr3···Gr1* open chains, with Gr1*
some symmetry equivalent of Gr1 and where `···' denotes hydrogen bonding. |
No. | Descriptor* | Gr1 | Gr2 | Gr3 |
1 | C2,2(8) | (H1WA-O1W-Ni1-O2W-H2WA) | (O2-S1-O4) | |
2 | C2,2(8) | (H1WB-O1W-Ni1-O2W-H2WA) | (O2-S1-O4) | |
3 | C2,2(8) | (H2WA-O2W-Ni1-O3W-H3WB) | (O4-S1-O2)i | |
4 | C2,2(8) | (H2WB-O2W-Ni1-O3W-H3WB) | (O4-S1-O3)i | |
5 | C1,2(6) | (H2WA-O2W-Ni1-O4W-H4WB) | O2ii | |
6 | C2,2(8) | (H2WB-O2W-Ni1-O4W-H4WB) | (O2-S1-O3)ii | |
7 | C2,2(8) | (H3WB-O3W-Ni1-O4W-H4WA) | (O1-S1-O4)iii | |
8 | C2,2(8) | (H1WA-O1W-Ni1-O4W-H4WA) | (O1-S1-O4)iii | |
9 | C2,2(8) | (H1WB-O1W-Ni1-O4W-H4WA) | (O1-S1-O4)iii | |
10 | C2,2(8) | (H1WA-O1W-Ni1-O2W-H2WB) | (O3-S1-O4)iii | |
11 | C2,2(8) | (H1WB-O1W-Ni1-O2W-H2WB) | (O3-S1-O4)iii | |
12 | C2,2(6) | (H4WB-O4W-H4WA) | (O1-S1-O2)iii | |
13 | C3,3(8) | (H3WB-O3W-H3WA) | (O5W-H5WB) | (O3-S1-O4) |
14 | C3,3(10) | (H1WA-O1W-Ni1-O3W-H3WA) | (O5W-H5WB) | (O3-S1-O4) |
15 | C3,3(10) | (H1WB-O1W-Ni1-O3W-H3WA) | (O5W-H5WB) | (O3-S1-O4) |
16 | C3,3(10) | (H4WB-O4W-Ni1-O3W-H3WA) | (O5W-H5WB) | (O3-S1-O2) |
17 | C3,3(10) | (H4WB-O4W-Ni1-O3W-H3WA) | (O5W-H5WA) | (O1-S1-O2)iii |
18 | C3,3(8) | (H3WB-O3W-H3WA) | (O5W-H5WA) | (O1-S1-O4)iii |
19 | C3,3(10) | (H1WA-O1W-Ni1-O3W-H3WA) | (O5W-H5WA) | (O1-S1-O4)iii |
20 | C3,3(10) | (H1WB-O1W-Ni1-O3W-H3WA) | (O5W-H5WA) | (O1-S1-O4)iii |
Notes: (*) for an introduction to graph-set analysis and notation, see
Bernstein et al. (1995) and Etter et al. (1990).
For a graph-set code
Xad(n), X is the structure code
(C = chain and R = ring), a is the total number of
acceptors involved, d is the total number of donors involved and
n is the total number of bonds involved.
Symmetry codes: (i) x + 1/2, -y + 1/2, z + 1/2; (ii)
-x + 3/2, y + 1/2, -z + 1/2; (iii) -x + 1,
-y + 1, -z; (iv) -x + 2, -y + 1, -z + 1. |
Supplementary Table S5. Hydrogen-bonded rings in (IIa), involving up to
three different primary hydrogen bonds between groups of atoms Gri topThe interactions have the form of Gr1···Gr2···Gr3···Gr1 closed loops, where
`···' denotes hydrogen bonding. |
No. | Descriptor* | Gr1 | Gr2 | Gr3 | Gr4 | Gr5 | Gr6 |
1 | R1,2(6) | (H1WA-O1W-Ni1-O3W-H3WB) | (O4)i | | | | |
2 | R2,2(8) | (H1WB-O1W-Ni1-O4W-H4WB) | (O2-S1-O4)ii | | | | |
3 | R2,2(8) | (H2WB-O2W-Ni1-O4W-H4WA) | (O1-S1-O3)iii | | | | |
4 | R3,3(8) | (H4WA-O4W-Ni1-O3W-H3WA) | (O5W-H5WA) | (O1)iii | | | |
5 | R3,3(10) | (H2WB-O2W-Ni1-O3W-H3WA) | (O5W-H5WA) | (O1-S1-O3)iii | | | |
6 | R3,3(10) | (H2WA-O2W-Ni1-O3W-H3WA) | (O5W-H5WB) | (O3-S1-O2) | | | |
7 | R2,4(8) | (H1WB-O1W-H1WA) | (O4)i | (H1WB-O1W-H1WA)iv | (O4)ii | | |
8 | R2,4(12) | (H1WB-O1W-Ni1-O3W-H3WB) | (O4)i | (H1WB-O1W-Ni1-O3W-H3WB)iv | (O4)ii | | |
9 | R4,4(12) | (H2WB-O2W-H2WA) | (O2-S1-O3) | (H2WB-O2W-H2WA)iii | (O2-S1-O3)iii | | |
10 | R4,4(12) | (H5WB-O5W-H5WA) | (O1-S1-O3)iii | (H5WB-O5W-H5WA)iii | (O1-S1-O3) | | |
11 | R4,4(16) | (H2WA-O2W-Ni1-O4W-H4WA) | (O1-S1-O2)iii | (H2WA-O2W-Ni1-O4W-H4WA)iii | (O1-S1-O2) | | |
12 | R4,4(16) | (H3WB-O3W-Ni1-O4W-H4WB) | (O2-S1-O4)ii | (H3WB-O3W-Ni1-O4W-H4WB)iv | (O2-S1-O4)i | | |
13 | R4,4(16) | (H1WA-O1W-Ni1-O4W-H4WB) | (O2-S1-O4)ii | (H1WA-O1W-Ni1-O4W-H4WB)iv | (O2-S1-O4)i | | |
14 | R4,6(16) | (H2WB-O2W-Ni1-O3W-H3WA) | (O5W-H5WB) | (O3) | (H2WB-O2W-Ni1-O3W-H3WA)iii | (O5W-H5WB)iii | (O3)iii |
15 | R6,6(20) | (H2WA-O2W-Ni1-O3W-H3WA) | (O5W-H5WA) | (O1-S1-O2)iii | (H2WA-O2W-Ni1-O3W-H3WA)iii | (O5W-H5WA)iii | (O1–S1-O2) |
16 | R6,6(20) | (H4WA-O4W-Ni1-O3W-H3WA) | (O5W-H5WB) | (O3-S1-O1) | (H4WA-O4W-Ni1-O3W-H3WA)iii | (O5W-H5WB)iii | (O3-S1-O1)iii |
Notes: (*) for an introduction to graph-set analysis and notation, see
Bernstein et al. (1995) and Etter et al. (1990).
For a graph-set code
Xad(n), X is the structure code
(C = chain and R = ring), a is the total number of
acceptors involved, d is the total number of donors involved and
n is the total number of bonds involved.
Symmetry codes: (i) x + 1/2, -y + 1/2, z + 1/2; (ii)
-x + 3/2, y + 1/2, -z + 1/2; (iii) -x + 1,
-y + 1, -z. |
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