The title compound, [Ni(chedam)(H2O)3]·1.5H2O [H2chedam = 4-hydroxypyridine-2,6-dicarboxylic acid, C7H5NO5], consists of one nickel cation, one chedam ligand, three coordinated water molecules and 1.5 uncoordinated water molecules. The nickel(II) cation is six-coordinate, with a distorted octahedral geometry.
Supporting information
CCDC reference: 620525
Key indicators
- Single-crystal X-ray study
- T = 294 K
- R factor = 0.068
- wR factor = 0.157
- Data-to-parameter ratio = 12.0
checkCIF/PLATON results
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Data collection: SMART (Bruker, 1997); cell refinement: SMART; data reduction: SAINT (Bruker, 1997); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Bruker, 1997); software used to prepare material for publication: SHELXTL.
triaqua(4-hydroxypyridine-2,6-dicarboxylato)nickel(II) sesquihydrate,
top
Crystal data top
[Ni(C7H3NO5)(H2O)3]·1.5H2O | F(000) = 1320 |
Mr = 320.89 | Dx = 1.827 Mg m−3 |
Monoclinic, C2/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -C 2yc | Cell parameters from 2877 reflections |
a = 14.879 (2) Å | θ = 2.7–26.2° |
b = 6.9505 (14) Å | µ = 1.71 mm−1 |
c = 22.567 (3) Å | T = 294 K |
β = 90.474 (9)° | Prism, green |
V = 2333.6 (7) Å3 | 0.22 × 0.18 × 0.12 mm |
Z = 8 | |
Data collection top
Bruker SMART CCD area-detector diffractometer | 2069 independent reflections |
Radiation source: fine-focus sealed tube | 1700 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.052 |
φ and ω scans | θmax = 25.0°, θmin = 1.8° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −17→16 |
Tmin = 0.698, Tmax = 0.821 | k = −8→8 |
5364 measured reflections | l = −26→19 |
Refinement top
Refinement on F2 | 0 restraints |
Least-squares matrix: full | H-atom parameters constrained |
R[F2 > 2σ(F2)] = 0.068 | w = 1/[σ2(Fo2) + (0.0372P)2 + 28.3869P] where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.157 | (Δ/σ)max = 0.001 |
S = 1.23 | Δρmax = 0.61 e Å−3 |
2069 reflections | Δρmin = −0.71 e Å−3 |
172 parameters | |
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. |
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. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | Occ. (<1) |
Ni1 | 0.47855 (6) | 0.24982 (13) | 0.63775 (3) | 0.0215 (3) | |
O1 | 0.5262 (3) | 0.2907 (6) | 0.54577 (18) | 0.0213 (10) | |
O2 | 0.4838 (3) | 0.2376 (7) | 0.45089 (18) | 0.0258 (10) | |
O3 | 0.3871 (3) | 0.1554 (7) | 0.70502 (18) | 0.0280 (11) | |
O4 | 0.2701 (4) | −0.0510 (9) | 0.7144 (2) | 0.0492 (16) | |
O5 | 0.1701 (3) | −0.0751 (6) | 0.48919 (18) | 0.0226 (10) | |
H5 | 0.1257 | −0.1138 | 0.5094 | 0.034* | |
O6 | 0.5530 (3) | −0.0065 (7) | 0.6445 (2) | 0.0317 (12) | |
H6A | 0.5580 | −0.0841 | 0.6156 | 0.038* | |
H6B | 0.5928 | 0.0042 | 0.6714 | 0.038* | |
O7 | 0.4237 (3) | 0.5276 (7) | 0.63416 (19) | 0.0274 (11) | |
H7A | 0.4226 | 0.5652 | 0.5984 | 0.033* | |
H7B | 0.3671 | 0.5309 | 0.6386 | 0.033* | |
O8 | 0.5735 (3) | 0.3641 (7) | 0.6927 (2) | 0.0294 (11) | |
H8A | 0.5887 | 0.2949 | 0.7222 | 0.035* | |
H8B | 0.5849 | 0.4790 | 0.7030 | 0.035* | |
N1 | 0.3823 (3) | 0.1284 (7) | 0.5886 (2) | 0.0205 (12) | |
C1 | 0.4712 (4) | 0.2279 (8) | 0.5058 (3) | 0.0179 (13) | |
C2 | 0.3853 (4) | 0.1341 (8) | 0.5294 (3) | 0.0141 (12) | |
C3 | 0.3147 (4) | 0.0618 (8) | 0.4948 (3) | 0.0153 (13) | |
H3 | 0.3179 | 0.0630 | 0.4536 | 0.018* | |
C4 | 0.2381 (4) | −0.0132 (8) | 0.5235 (3) | 0.0163 (13) | |
C5 | 0.2373 (4) | −0.0216 (9) | 0.5859 (3) | 0.0206 (14) | |
H5A | 0.1886 | −0.0743 | 0.6058 | 0.025* | |
C6 | 0.3111 (4) | 0.0510 (9) | 0.6171 (3) | 0.0203 (14) | |
C7 | 0.3220 (5) | 0.0547 (10) | 0.6846 (3) | 0.0277 (16) | |
O9 | 0.7372 (4) | 0.0536 (8) | 0.6682 (2) | 0.0381 (13) | |
H9A | 0.7383 | −0.0021 | 0.7018 | 0.046* | |
H9B | 0.7463 | 0.1666 | 0.6814 | 0.046* | |
O10 | 0.5176 (13) | 0.7121 (14) | 0.7491 (15) | 0.060 (5) | 0.50 |
H10A | 0.5341 | 0.6611 | 0.7817 | 0.089* | 0.50 |
H10B | 0.5637 | 0.7406 | 0.7286 | 0.089* | 0.50 |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Ni1 | 0.0198 (4) | 0.0260 (4) | 0.0186 (4) | −0.0056 (4) | −0.0041 (3) | −0.0006 (4) |
O1 | 0.016 (2) | 0.023 (3) | 0.024 (2) | −0.0048 (18) | −0.0011 (18) | −0.0018 (18) |
O2 | 0.024 (2) | 0.032 (3) | 0.022 (2) | −0.015 (2) | 0.0050 (18) | −0.004 (2) |
O3 | 0.029 (3) | 0.037 (3) | 0.018 (2) | −0.013 (2) | −0.0033 (19) | −0.003 (2) |
O4 | 0.044 (3) | 0.078 (4) | 0.026 (3) | −0.035 (3) | 0.001 (2) | −0.001 (3) |
O5 | 0.016 (2) | 0.030 (3) | 0.022 (2) | −0.009 (2) | −0.0035 (18) | 0.001 (2) |
O6 | 0.042 (3) | 0.028 (3) | 0.025 (2) | 0.006 (2) | −0.012 (2) | −0.006 (2) |
O7 | 0.026 (3) | 0.033 (3) | 0.023 (2) | −0.001 (2) | 0.0016 (19) | 0.004 (2) |
O8 | 0.028 (3) | 0.032 (3) | 0.028 (3) | −0.013 (2) | −0.010 (2) | 0.001 (2) |
N1 | 0.021 (3) | 0.025 (3) | 0.016 (3) | −0.003 (2) | 0.001 (2) | −0.002 (2) |
C1 | 0.014 (3) | 0.015 (3) | 0.024 (3) | −0.003 (3) | −0.003 (2) | −0.002 (3) |
C2 | 0.009 (3) | 0.013 (3) | 0.020 (3) | 0.000 (2) | 0.004 (2) | 0.001 (2) |
C3 | 0.012 (3) | 0.019 (3) | 0.015 (3) | −0.004 (3) | −0.001 (2) | 0.001 (2) |
C4 | 0.013 (3) | 0.010 (3) | 0.026 (3) | 0.004 (2) | −0.004 (2) | −0.004 (2) |
C5 | 0.014 (3) | 0.023 (3) | 0.026 (3) | −0.001 (3) | 0.006 (3) | 0.000 (3) |
C6 | 0.023 (3) | 0.017 (3) | 0.020 (3) | −0.005 (3) | −0.002 (3) | 0.002 (3) |
C7 | 0.029 (4) | 0.033 (4) | 0.021 (3) | −0.014 (3) | 0.006 (3) | 0.000 (3) |
O9 | 0.040 (3) | 0.046 (3) | 0.029 (3) | −0.003 (3) | −0.001 (2) | 0.003 (2) |
O10 | 0.068 (12) | 0.049 (6) | 0.062 (6) | 0.001 (6) | −0.010 (9) | 0.007 (7) |
Geometric parameters (Å, º) top
Ni1—N1 | 1.993 (5) | O8—H8B | 0.8484 |
Ni1—O8 | 2.034 (4) | N1—C2 | 1.337 (7) |
Ni1—O7 | 2.097 (5) | N1—C6 | 1.355 (8) |
Ni1—O6 | 2.103 (5) | C1—C2 | 1.534 (8) |
Ni1—O3 | 2.149 (5) | C2—C3 | 1.398 (8) |
Ni1—O1 | 2.217 (4) | C3—C4 | 1.415 (8) |
O1—C1 | 1.289 (7) | C3—H3 | 0.9300 |
O2—C1 | 1.257 (7) | C4—C5 | 1.409 (9) |
O3—C7 | 1.279 (8) | C5—C6 | 1.395 (9) |
O4—C7 | 1.263 (8) | C5—H5A | 0.9300 |
O5—C4 | 1.340 (7) | C6—C7 | 1.529 (9) |
O5—H5 | 0.8494 | O9—H9A | 0.8509 |
O6—H6A | 0.8493 | O9—H9B | 0.8508 |
O6—H6B | 0.8479 | O10—O10i | 0.53 (4) |
O7—H7A | 0.8488 | O10—H10A | 0.8509 |
O7—H7B | 0.8497 | O10—H10B | 0.8544 |
O8—H8A | 0.8507 | | |
| | | |
N1—Ni1—O8 | 176.2 (2) | C2—N1—Ni1 | 120.9 (4) |
N1—Ni1—O7 | 95.2 (2) | C6—N1—Ni1 | 117.6 (4) |
O8—Ni1—O7 | 86.11 (19) | O2—C1—O1 | 124.9 (6) |
N1—Ni1—O6 | 93.3 (2) | O2—C1—C2 | 119.8 (5) |
O8—Ni1—O6 | 85.6 (2) | O1—C1—C2 | 115.3 (5) |
O7—Ni1—O6 | 170.87 (19) | N1—C2—C3 | 121.1 (5) |
N1—Ni1—O3 | 78.92 (18) | N1—C2—C1 | 113.2 (5) |
O8—Ni1—O3 | 97.41 (18) | C3—C2—C1 | 125.7 (5) |
O7—Ni1—O3 | 93.44 (19) | C2—C3—C4 | 118.7 (5) |
O6—Ni1—O3 | 91.5 (2) | C2—C3—H3 | 120.6 |
N1—Ni1—O1 | 76.53 (18) | C4—C3—H3 | 120.6 |
O8—Ni1—O1 | 107.15 (17) | O5—C4—C5 | 123.4 (6) |
O7—Ni1—O1 | 88.48 (16) | O5—C4—C3 | 117.4 (5) |
O6—Ni1—O1 | 90.23 (17) | C5—C4—C3 | 119.2 (5) |
O3—Ni1—O1 | 155.44 (16) | C6—C5—C4 | 118.5 (6) |
C1—O1—Ni1 | 113.9 (4) | C6—C5—H5A | 120.8 |
C7—O3—Ni1 | 113.3 (4) | C4—C5—H5A | 120.8 |
C4—O5—H5 | 112.2 | N1—C6—C5 | 121.2 (5) |
Ni1—O6—H6A | 122.1 | N1—C6—C7 | 113.0 (5) |
Ni1—O6—H6B | 110.0 | C5—C6—C7 | 125.8 (6) |
H6A—O6—H6B | 122.7 | O4—C7—O3 | 126.3 (6) |
Ni1—O7—H7A | 108.9 | O4—C7—C6 | 117.4 (6) |
Ni1—O7—H7B | 114.0 | O3—C7—C6 | 116.2 (5) |
H7A—O7—H7B | 95.4 | H9A—O9—H9B | 96.1 |
Ni1—O8—H8A | 115.8 | O10i—O10—H10A | 102.4 |
Ni1—O8—H8B | 132.2 | O10i—O10—H10B | 147.8 |
H8A—O8—H8B | 105.4 | H10A—O10—H10B | 109.8 |
C2—N1—C6 | 121.3 (5) | | |
| | | |
N1—Ni1—O1—C1 | 2.6 (4) | Ni1—N1—C2—C1 | 4.0 (7) |
O8—Ni1—O1—C1 | −178.6 (4) | O2—C1—C2—N1 | 177.9 (5) |
O7—Ni1—O1—C1 | −93.1 (4) | O1—C1—C2—N1 | −1.5 (8) |
O6—Ni1—O1—C1 | 95.9 (4) | O2—C1—C2—C3 | −2.9 (9) |
O3—Ni1—O1—C1 | 1.8 (7) | O1—C1—C2—C3 | 177.7 (5) |
N1—Ni1—O3—C7 | 6.2 (5) | N1—C2—C3—C4 | 1.8 (9) |
O8—Ni1—O3—C7 | −172.6 (5) | C1—C2—C3—C4 | −177.3 (5) |
O7—Ni1—O3—C7 | 100.8 (5) | C2—C3—C4—O5 | 177.7 (5) |
O6—Ni1—O3—C7 | −86.9 (5) | C2—C3—C4—C5 | −3.1 (8) |
O1—Ni1—O3—C7 | 7.0 (8) | O5—C4—C5—C6 | −178.6 (6) |
O7—Ni1—N1—C2 | 83.5 (5) | C3—C4—C5—C6 | 2.2 (9) |
O6—Ni1—N1—C2 | −93.1 (5) | C2—N1—C6—C5 | −1.5 (9) |
O3—Ni1—N1—C2 | 176.0 (5) | Ni1—N1—C6—C5 | 174.4 (5) |
O1—Ni1—N1—C2 | −3.6 (4) | C2—N1—C6—C7 | 178.7 (6) |
O7—Ni1—N1—C6 | −92.4 (5) | Ni1—N1—C6—C7 | −5.4 (7) |
O6—Ni1—N1—C6 | 91.0 (5) | C4—C5—C6—N1 | 0.1 (9) |
O3—Ni1—N1—C6 | 0.1 (5) | C4—C5—C6—C7 | 179.8 (6) |
O1—Ni1—N1—C6 | −179.5 (5) | Ni1—O3—C7—O4 | 164.2 (7) |
Ni1—O1—C1—O2 | 179.3 (5) | Ni1—O3—C7—C6 | −10.8 (8) |
Ni1—O1—C1—C2 | −1.3 (6) | N1—C6—C7—O4 | −164.4 (7) |
C6—N1—C2—C3 | 0.6 (9) | C5—C6—C7—O4 | 15.9 (11) |
Ni1—N1—C2—C3 | −175.2 (4) | N1—C6—C7—O3 | 11.0 (9) |
C6—N1—C2—C1 | 179.8 (5) | C5—C6—C7—O3 | −168.7 (7) |
Symmetry code: (i) −x+1, y, −z+3/2. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O5—H5···O1ii | 0.85 | 1.82 | 2.670 (6) | 174 |
O6—H6A···O2iii | 0.85 | 1.94 | 2.738 (6) | 156 |
O7—H7A···O2iv | 0.85 | 2.25 | 2.878 (6) | 131 |
O7—H7A···O5v | 0.85 | 2.40 | 3.121 (6) | 143 |
O8—H8A···O3i | 0.85 | 1.94 | 2.784 (6) | 173 |
Symmetry codes: (i) −x+1, y, −z+3/2; (ii) x−1/2, y−1/2, z; (iii) −x+1, −y, −z+1; (iv) −x+1, −y+1, −z+1; (v) −x+1/2, −y+1/2, −z+1. |