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In the title compound, [Ni(HQS)(H
2O)
4]·H
2O (HQS is the 8-hydroxyquinoline-5-sulfonic acid dianion, C
9H
13NO
8S), the Ni
II ion is coordinated by the N and quinolinolate-O atoms of HQS and four water molecules, exhibiting a distorted octahedral geometry. The sulfonic O atoms of HQS are not involved in the coordination. However, the sulfonic O atoms along with the coordinated and lattice water molecules play a vital role in assembling the three-dimensional structure by an extensive network of intermolecular O—H
O hydrogen bonds. Furthermore, the overall structure is stabilized by π–π stacking interactions between the ring moieties of HQS in the neighbouring complex molecules.
Supporting information
CCDC reference: 166282
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (C-C) = 0.002 Å
- R factor = 0.023
- wR factor = 0.062
- Data-to-parameter ratio = 12.8
checkCIF results
No syntax errors found
ADDSYM reports no extra symmetry
Alert Level C:
REFLT_03
From the CIF: _diffrn_reflns_theta_max 28.05
From the CIF: _reflns_number_total 3222
TEST2: Reflns within _diffrn_reflns_theta_max
Count of symmetry unique reflns 3445
Completeness (_total/calc) 93.53%
Alert C: < 95% complete
0 Alert Level A = Potentially serious problem
0 Alert Level B = Potential problem
1 Alert Level C = Please check
Data collection: MolEN (Fair, 1990); cell refinement: MolEN; data reduction: MolEN; program(s) used to solve structure: SIR97 (Altomare et al., 1999); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: PLATON97 (Spek, 1997); software used to prepare material for publication: PLATON97.
'[Tetraaqua(quinolinolato-
N,
O]-5-sulfonic nickel(II)]monohydrate'
top
Crystal data top
[Ni(C9H13NO8S)]·H2O | F(000) = 768 |
Mr = 371.99 | Dx = 1.741 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71069 Å |
Hall symbol: -P 2yn | Cell parameters from 25 reflections |
a = 7.366 (2) Å | θ = 1.9–28.0° |
b = 9.000 (2) Å | µ = 1.56 mm−1 |
c = 21.456 (2) Å | T = 293 K |
β = 93.73 (2)° | Prism, green |
V = 1419.4 (5) Å3 | 0.36 × 0.29 × 0.25 mm |
Z = 4 | |
Data collection top
Bruker AXS SMART diffractometer | 3222 independent reflections |
Radiation source: fine-ficus sealed tube | 2925 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.023 |
ω–2θ scans | θmax = 28.1°, θmin = 1.9° |
Absorption correction: ψ scan (North et al., 1968) | h = −9→9 |
Tmin = 0.519, Tmax = 0.678 | k = −11→11 |
14764 measured reflections | l = −28→28 |
Refinement top
Refinement on F2 | 0 restraints |
Least-squares matrix: full | All H-atom parameters refined |
R[F2 > 2σ(F2)] = 0.023 | w = 1/[σ2(Fo2) + (0.0377P)2 + 0.402P] where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.062 | (Δ/σ)max = 0.009 |
S = 1.02 | Δρmax = 0.13 e Å−3 |
3222 reflections | Δρmin = −0.10 e Å−3 |
251 parameters | |
Special details top
Geometry. Bond distances, angles etc. have been calculated using the rounded
fractional coordinates. All e.s.d.'s are estimated from the variances of the
(full) variance-covariance matrix. The cell e.s.d.'s are taken into account in
the estimation of distances, angles and torsion angles |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Ni1 | 0.14810 (3) | 0.23203 (2) | 0.44408 (1) | 0.0234 (1) | |
S17 | −0.09951 (5) | 0.03912 (4) | 0.13820 (2) | 0.0252 (1) | |
O2 | 0.25729 (19) | 0.43254 (14) | 0.47382 (6) | 0.0340 (4) | |
O3 | 0.41182 (17) | 0.16353 (15) | 0.42669 (7) | 0.0348 (4) | |
O4 | −0.10412 (16) | 0.31460 (14) | 0.46637 (6) | 0.0313 (3) | |
O5 | 0.18929 (17) | 0.15168 (14) | 0.53371 (5) | 0.0315 (3) | |
O6 | 0.05801 (15) | 0.03199 (12) | 0.41243 (5) | 0.0275 (3) | |
O18 | −0.12771 (16) | −0.11759 (13) | 0.12173 (5) | 0.0333 (4) | |
O19 | 0.05744 (16) | 0.10137 (14) | 0.10897 (5) | 0.0345 (4) | |
O20 | −0.26216 (16) | 0.12715 (14) | 0.12556 (5) | 0.0356 (4) | |
N7 | 0.09165 (17) | 0.28958 (14) | 0.35164 (6) | 0.0245 (3) | |
C8 | 0.0987 (2) | 0.42023 (17) | 0.32393 (8) | 0.0297 (5) | |
C9 | 0.0583 (3) | 0.43781 (18) | 0.25937 (8) | 0.0333 (5) | |
C10 | 0.0113 (2) | 0.31748 (18) | 0.22336 (7) | 0.0298 (5) | |
C11 | 0.0010 (2) | 0.17478 (16) | 0.25149 (7) | 0.0241 (4) | |
C12 | −0.0463 (2) | 0.04052 (16) | 0.21937 (7) | 0.0248 (4) | |
C13 | −0.0524 (2) | −0.09077 (18) | 0.25230 (8) | 0.0297 (5) | |
C14 | −0.0148 (2) | −0.09687 (17) | 0.31715 (7) | 0.0307 (5) | |
C15 | 0.0290 (2) | 0.03031 (16) | 0.35102 (7) | 0.0246 (4) | |
C16 | 0.04154 (19) | 0.16756 (16) | 0.31690 (7) | 0.0228 (4) | |
O1 | 0.1686 (2) | 0.34024 (17) | 0.03504 (7) | 0.0410 (4) | |
H2 | 0.322 (3) | 0.481 (3) | 0.4524 (12) | 0.056 (7)* | |
H2' | 0.199 (4) | 0.493 (3) | 0.4902 (12) | 0.057 (7)* | |
H3 | 0.468 (4) | 0.222 (3) | 0.4062 (13) | 0.062 (8)* | |
H3' | 0.465 (4) | 0.149 (3) | 0.4579 (14) | 0.071 (9)* | |
H4 | −0.155 (4) | 0.261 (3) | 0.4878 (13) | 0.057 (8)* | |
H4' | −0.166 (3) | 0.332 (3) | 0.4343 (13) | 0.060 (7)* | |
H5 | 0.108 (3) | 0.098 (3) | 0.5469 (11) | 0.050 (6)* | |
H5' | 0.219 (3) | 0.217 (3) | 0.5628 (13) | 0.057 (7)* | |
H8 | 0.135 (2) | 0.504 (2) | 0.3498 (8) | 0.027 (4)* | |
H9 | 0.063 (3) | 0.533 (2) | 0.2401 (10) | 0.043 (5)* | |
H10 | −0.015 (3) | 0.329 (2) | 0.1786 (10) | 0.038 (5)* | |
H13 | −0.090 (3) | −0.181 (2) | 0.2304 (9) | 0.036 (5)* | |
H14 | −0.019 (3) | −0.186 (2) | 0.3396 (10) | 0.046 (6)* | |
H1 | 0.125 (4) | 0.294 (3) | 0.0586 (14) | 0.063 (9)* | |
H1' | 0.225 (4) | 0.396 (3) | 0.0519 (12) | 0.058 (8)* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Ni1 | 0.0284 (1) | 0.0235 (1) | 0.0182 (1) | −0.0034 (1) | 0.0002 (1) | 0.0000 (1) |
S17 | 0.0299 (2) | 0.0271 (2) | 0.0184 (2) | 0.0044 (1) | −0.0006 (1) | −0.0034 (1) |
O2 | 0.0446 (7) | 0.0278 (6) | 0.0305 (6) | −0.0090 (5) | 0.0102 (5) | −0.0051 (5) |
O3 | 0.0315 (6) | 0.0353 (7) | 0.0377 (7) | −0.0024 (5) | 0.0031 (6) | 0.0061 (5) |
O4 | 0.0310 (6) | 0.0364 (6) | 0.0263 (6) | 0.0018 (5) | 0.0014 (5) | 0.0037 (5) |
O5 | 0.0394 (7) | 0.0340 (6) | 0.0210 (5) | −0.0083 (5) | 0.0002 (5) | 0.0026 (5) |
O6 | 0.0372 (6) | 0.0261 (5) | 0.0188 (5) | −0.0066 (4) | −0.0006 (4) | 0.0022 (4) |
O18 | 0.0421 (7) | 0.0295 (6) | 0.0275 (6) | 0.0039 (5) | −0.0050 (5) | −0.0087 (5) |
O19 | 0.0386 (6) | 0.0402 (7) | 0.0253 (6) | 0.0010 (5) | 0.0070 (5) | 0.0002 (5) |
O20 | 0.0378 (6) | 0.0393 (7) | 0.0292 (6) | 0.0133 (5) | −0.0014 (5) | −0.0001 (5) |
N7 | 0.0280 (6) | 0.0239 (6) | 0.0214 (6) | −0.0029 (5) | 0.0000 (5) | −0.0007 (5) |
C8 | 0.0383 (9) | 0.0231 (7) | 0.0271 (8) | −0.0038 (6) | −0.0015 (6) | −0.0011 (6) |
C9 | 0.0445 (10) | 0.0240 (8) | 0.0308 (8) | −0.0027 (7) | −0.0020 (7) | 0.0056 (6) |
C10 | 0.0390 (9) | 0.0283 (8) | 0.0220 (8) | 0.0006 (7) | 0.0001 (6) | 0.0041 (6) |
C11 | 0.0258 (7) | 0.0255 (7) | 0.0212 (7) | 0.0001 (6) | 0.0022 (5) | −0.0002 (6) |
C12 | 0.0281 (7) | 0.0277 (7) | 0.0184 (7) | 0.0001 (6) | 0.0005 (5) | −0.0013 (5) |
C13 | 0.0383 (9) | 0.0246 (7) | 0.0261 (8) | −0.0045 (6) | 0.0014 (6) | −0.0044 (6) |
C14 | 0.0447 (9) | 0.0225 (7) | 0.0249 (8) | −0.0060 (7) | 0.0026 (7) | 0.0016 (6) |
C15 | 0.0271 (7) | 0.0262 (7) | 0.0206 (7) | −0.0033 (6) | 0.0016 (5) | 0.0021 (5) |
C16 | 0.0246 (7) | 0.0234 (7) | 0.0205 (7) | −0.0018 (5) | 0.0019 (5) | −0.0010 (5) |
O1 | 0.0498 (8) | 0.0353 (7) | 0.0382 (7) | −0.0066 (6) | 0.0060 (6) | −0.0056 (6) |
Geometric parameters (Å, º) top
Ni1—O2 | 2.0601 (14) | O1—H1 | 0.74 (3) |
Ni1—O3 | 2.0945 (14) | O1—H1' | 0.73 (3) |
Ni1—O4 | 2.0852 (13) | N7—C8 | 1.320 (2) |
Ni1—O5 | 2.0585 (12) | N7—C16 | 1.365 (2) |
Ni1—O6 | 2.0209 (12) | C8—C9 | 1.407 (2) |
Ni1—N7 | 2.0658 (14) | C9—C10 | 1.362 (2) |
S17—O18 | 1.4655 (13) | C10—C11 | 1.423 (2) |
S17—O19 | 1.4622 (13) | C11—C12 | 1.423 (2) |
S17—O20 | 1.4472 (13) | C11—C16 | 1.417 (2) |
S17—C12 | 1.7601 (16) | C12—C13 | 1.379 (2) |
O6—C15 | 1.3211 (19) | C13—C14 | 1.402 (2) |
O2—H2 | 0.81 (2) | C14—C15 | 1.383 (2) |
O2—H2' | 0.79 (3) | C15—C16 | 1.442 (2) |
O3—H3' | 0.76 (3) | C8—H8 | 0.964 (18) |
O3—H3 | 0.82 (3) | C9—H9 | 0.953 (19) |
O4—H4' | 0.82 (3) | C10—H10 | 0.97 (2) |
O4—H4 | 0.78 (3) | C13—H13 | 0.970 (18) |
O5—H5 | 0.83 (2) | C14—H14 | 0.937 (19) |
O5—H5' | 0.87 (3) | | |
| | | |
O2—Ni1—O3 | 88.00 (6) | Ni1—O5—H5 | 117.1 (16) |
O2—Ni1—O4 | 87.28 (6) | H1—O1—H1' | 108 (3) |
O2—Ni1—O5 | 89.28 (5) | C8—N7—C16 | 119.21 (14) |
O2—Ni1—O6 | 175.96 (5) | Ni1—N7—C16 | 110.67 (10) |
O2—Ni1—N7 | 97.35 (5) | Ni1—N7—C8 | 130.12 (11) |
O3—Ni1—O4 | 175.02 (6) | N7—C8—C9 | 122.12 (15) |
O3—Ni1—O5 | 88.91 (6) | C8—C9—C10 | 119.93 (15) |
O3—Ni1—O6 | 88.05 (5) | C9—C10—C11 | 119.71 (14) |
O3—Ni1—N7 | 91.94 (6) | C10—C11—C12 | 125.38 (14) |
O4—Ni1—O5 | 89.44 (5) | C12—C11—C16 | 118.02 (13) |
O4—Ni1—O6 | 96.69 (5) | C10—C11—C16 | 116.60 (13) |
O4—Ni1—N7 | 90.24 (5) | S17—C12—C13 | 119.23 (12) |
O5—Ni1—O6 | 91.50 (5) | S17—C12—C11 | 121.13 (11) |
O5—Ni1—N7 | 173.34 (5) | C11—C12—C13 | 119.64 (14) |
O6—Ni1—N7 | 81.93 (5) | C12—C13—C14 | 122.08 (15) |
O18—S17—O19 | 111.65 (7) | C13—C14—C15 | 120.90 (14) |
O18—S17—O20 | 112.27 (7) | C14—C15—C16 | 117.57 (14) |
O18—S17—C12 | 105.33 (7) | O6—C15—C14 | 123.42 (14) |
O19—S17—O20 | 112.20 (7) | O6—C15—C16 | 119.01 (13) |
O19—S17—C12 | 106.87 (7) | N7—C16—C15 | 115.85 (13) |
O20—S17—C12 | 108.05 (7) | N7—C16—C11 | 122.42 (13) |
Ni1—O6—C15 | 111.94 (9) | C11—C16—C15 | 121.72 (13) |
H2—O2—H2' | 104 (3) | C9—C8—H8 | 120.8 (10) |
Ni1—O2—H2 | 121.9 (19) | N7—C8—H8 | 117.1 (10) |
Ni1—O2—H2' | 122 (2) | C8—C9—H9 | 121.1 (13) |
Ni1—O3—H3 | 115 (2) | C10—C9—H9 | 118.9 (13) |
Ni1—O3—H3' | 109 (2) | C11—C10—H10 | 120.1 (11) |
H3—O3—H3' | 109 (3) | C9—C10—H10 | 120.1 (11) |
Ni1—O4—H4 | 113 (2) | C12—C13—H13 | 119.2 (11) |
H4—O4—H4' | 111 (3) | C14—C13—H13 | 118.7 (11) |
Ni1—O4—H4' | 109.4 (17) | C13—C14—H14 | 122.2 (13) |
Ni1—O5—H5' | 116.4 (18) | C15—C14—H14 | 116.9 (13) |
H5—O5—H5' | 107 (2) | | |
| | | |
O3—Ni1—O6—C15 | −85.26 (10) | Ni1—N7—C16—C15 | 3.17 (16) |
O4—Ni1—O6—C15 | 96.27 (10) | C16—N7—C8—C9 | −0.8 (2) |
O5—Ni1—O6—C15 | −174.12 (10) | N7—C8—C9—C10 | −0.5 (3) |
N7—Ni1—O6—C15 | 6.98 (10) | C8—C9—C10—C11 | 0.8 (3) |
O2—Ni1—N7—C8 | −8.99 (14) | C9—C10—C11—C12 | 180.00 (16) |
O2—Ni1—N7—C16 | 170.54 (10) | C9—C10—C11—C16 | 0.0 (2) |
O3—Ni1—N7—C8 | −97.22 (14) | C10—C11—C12—S17 | −0.2 (2) |
O3—Ni1—N7—C16 | 82.31 (10) | C12—C11—C16—C15 | −2.4 (2) |
O4—Ni1—N7—C8 | 78.30 (14) | C10—C11—C12—C13 | −179.61 (15) |
O4—Ni1—N7—C16 | −102.17 (10) | C10—C11—C16—C15 | 177.59 (14) |
O6—Ni1—N7—C8 | 175.03 (14) | C12—C11—C16—N7 | 178.73 (14) |
O6—Ni1—N7—C16 | −5.44 (10) | C16—C11—C12—C13 | 0.4 (2) |
O18—S17—C12—C13 | −4.49 (14) | C10—C11—C16—N7 | −1.3 (2) |
O19—S17—C12—C13 | −123.37 (13) | C16—C11—C12—S17 | 179.77 (11) |
O20—S17—C12—C13 | 115.69 (13) | S17—C12—C13—C14 | −178.83 (12) |
O20—S17—C12—C11 | −63.70 (14) | C11—C12—C13—C14 | 0.6 (2) |
O18—S17—C12—C11 | 176.12 (12) | C12—C13—C14—C15 | 0.5 (2) |
O19—S17—C12—C11 | 57.25 (14) | C13—C14—C15—C16 | −2.4 (2) |
Ni1—O6—C15—C14 | 173.08 (12) | C13—C14—C15—O6 | 177.01 (14) |
Ni1—O6—C15—C16 | −7.50 (17) | O6—C15—C16—N7 | 2.9 (2) |
Ni1—N7—C16—C11 | −177.90 (11) | O6—C15—C16—C11 | −176.04 (13) |
Ni1—N7—C8—C9 | 178.69 (13) | C14—C15—C16—N7 | −177.65 (13) |
C8—N7—C16—C11 | 1.7 (2) | C14—C15—C16—C11 | 3.4 (2) |
C8—N7—C16—C15 | −177.24 (13) | | |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O1—H1···O19 | 0.74 (3) | 2.12 (3) | 2.824 (2) | 159 (3) |
O1—H1′···O6i | 0.73 (3) | 2.12 (3) | 2.830 (2) | 165 (3) |
O2—H2···O19i | 0.81 (2) | 1.96 (3) | 2.7644 (19) | 170 (2) |
O2—H2′···O4ii | 0.79 (3) | 2.11 (3) | 2.879 (2) | 166 (3) |
O3—H3···O18i | 0.82 (3) | 1.98 (3) | 2.7756 (19) | 165 (3) |
O3—H3′···O1iii | 0.76 (3) | 2.16 (3) | 2.900 (2) | 162 (3) |
O4—H4···O1iv | 0.78 (3) | 1.93 (3) | 2.690 (2) | 166 (3) |
O4—H4′···O18v | 0.82 (3) | 1.93 (2) | 2.7133 (18) | 161 (2) |
O5—H5···O6vi | 0.83 (2) | 1.94 (2) | 2.7677 (18) | 172 (2) |
O5—H5′···O20iii | 0.87 (3) | 1.94 (3) | 2.8075 (18) | 169 (2) |
C8—H8···O19i | 0.964 (18) | 2.534 (16) | 3.267 (2) | 132.8 (12) |
C13—H13···O18 | 0.970 (18) | 2.399 (19) | 2.831 (2) | 106.4 (13) |
C14—H14···O20vii | 0.937 (19) | 2.48 (2) | 3.262 (2) | 141.2 (18) |
Symmetry codes: (i) −x+1/2, y+1/2, −z+1/2; (ii) −x, −y+1, −z+1; (iii) x+1/2, −y+1/2, z+1/2; (iv) x−1/2, −y+1/2, z+1/2; (v) −x−1/2, y+1/2, −z+1/2; (vi) −x, −y, −z+1; (vii) −x−1/2, y−1/2, −z+1/2. |
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