Buy article online - an online subscription or single-article purchase is required to access this article.
Download citation
Download citation
link to html
In the title compound, [Ni(HQS)(H2O)4]·H2O (HQS is the 8-hydroxy­quinoline-5-sulfonic acid dianion, C9H13NO8S), the NiII 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

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536801017792/ob6080sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536801017792/ob6080Isup2.hkl
Contains datablock I

CCDC reference: 166282

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](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


Yellow Alert 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

Computing details top

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)]·H2OF(000) = 768
Mr = 371.99Dx = 1.741 Mg m3
Monoclinic, P21/nMo Kα radiation, λ = 0.71069 Å
Hall symbol: -P 2ynCell parameters from 25 reflections
a = 7.366 (2) Åθ = 1.9–28.0°
b = 9.000 (2) ŵ = 1.56 mm1
c = 21.456 (2) ÅT = 293 K
β = 93.73 (2)°Prism, green
V = 1419.4 (5) Å30.36 × 0.29 × 0.25 mm
Z = 4
Data collection top
Bruker AXS SMART
diffractometer
3222 independent reflections
Radiation source: fine-ficus sealed tube2925 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.023
ω–2θ scansθmax = 28.1°, θmin = 1.9°
Absorption correction: ψ scan
(North et al., 1968)
h = 99
Tmin = 0.519, Tmax = 0.678k = 1111
14764 measured reflectionsl = 2828
Refinement top
Refinement on F20 restraints
Least-squares matrix: fullAll 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 = 1.02Δρmax = 0.13 e Å3
3222 reflectionsΔρmin = 0.10 e Å3
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
xyzUiso*/Ueq
Ni10.14810 (3)0.23203 (2)0.44408 (1)0.0234 (1)
S170.09951 (5)0.03912 (4)0.13820 (2)0.0252 (1)
O20.25729 (19)0.43254 (14)0.47382 (6)0.0340 (4)
O30.41182 (17)0.16353 (15)0.42669 (7)0.0348 (4)
O40.10412 (16)0.31460 (14)0.46637 (6)0.0313 (3)
O50.18929 (17)0.15168 (14)0.53371 (5)0.0315 (3)
O60.05801 (15)0.03199 (12)0.41243 (5)0.0275 (3)
O180.12771 (16)0.11759 (13)0.12173 (5)0.0333 (4)
O190.05744 (16)0.10137 (14)0.10897 (5)0.0345 (4)
O200.26216 (16)0.12715 (14)0.12556 (5)0.0356 (4)
N70.09165 (17)0.28958 (14)0.35164 (6)0.0245 (3)
C80.0987 (2)0.42023 (17)0.32393 (8)0.0297 (5)
C90.0583 (3)0.43781 (18)0.25937 (8)0.0333 (5)
C100.0113 (2)0.31748 (18)0.22336 (7)0.0298 (5)
C110.0010 (2)0.17478 (16)0.25149 (7)0.0241 (4)
C120.0463 (2)0.04052 (16)0.21937 (7)0.0248 (4)
C130.0524 (2)0.09077 (18)0.25230 (8)0.0297 (5)
C140.0148 (2)0.09687 (17)0.31715 (7)0.0307 (5)
C150.0290 (2)0.03031 (16)0.35102 (7)0.0246 (4)
C160.04154 (19)0.16756 (16)0.31690 (7)0.0228 (4)
O10.1686 (2)0.34024 (17)0.03504 (7)0.0410 (4)
H20.322 (3)0.481 (3)0.4524 (12)0.056 (7)*
H2'0.199 (4)0.493 (3)0.4902 (12)0.057 (7)*
H30.468 (4)0.222 (3)0.4062 (13)0.062 (8)*
H3'0.465 (4)0.149 (3)0.4579 (14)0.071 (9)*
H40.155 (4)0.261 (3)0.4878 (13)0.057 (8)*
H4'0.166 (3)0.332 (3)0.4343 (13)0.060 (7)*
H50.108 (3)0.098 (3)0.5469 (11)0.050 (6)*
H5'0.219 (3)0.217 (3)0.5628 (13)0.057 (7)*
H80.135 (2)0.504 (2)0.3498 (8)0.027 (4)*
H90.063 (3)0.533 (2)0.2401 (10)0.043 (5)*
H100.015 (3)0.329 (2)0.1786 (10)0.038 (5)*
H130.090 (3)0.181 (2)0.2304 (9)0.036 (5)*
H140.019 (3)0.186 (2)0.3396 (10)0.046 (6)*
H10.125 (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
U11U22U33U12U13U23
Ni10.0284 (1)0.0235 (1)0.0182 (1)0.0034 (1)0.0002 (1)0.0000 (1)
S170.0299 (2)0.0271 (2)0.0184 (2)0.0044 (1)0.0006 (1)0.0034 (1)
O20.0446 (7)0.0278 (6)0.0305 (6)0.0090 (5)0.0102 (5)0.0051 (5)
O30.0315 (6)0.0353 (7)0.0377 (7)0.0024 (5)0.0031 (6)0.0061 (5)
O40.0310 (6)0.0364 (6)0.0263 (6)0.0018 (5)0.0014 (5)0.0037 (5)
O50.0394 (7)0.0340 (6)0.0210 (5)0.0083 (5)0.0002 (5)0.0026 (5)
O60.0372 (6)0.0261 (5)0.0188 (5)0.0066 (4)0.0006 (4)0.0022 (4)
O180.0421 (7)0.0295 (6)0.0275 (6)0.0039 (5)0.0050 (5)0.0087 (5)
O190.0386 (6)0.0402 (7)0.0253 (6)0.0010 (5)0.0070 (5)0.0002 (5)
O200.0378 (6)0.0393 (7)0.0292 (6)0.0133 (5)0.0014 (5)0.0001 (5)
N70.0280 (6)0.0239 (6)0.0214 (6)0.0029 (5)0.0000 (5)0.0007 (5)
C80.0383 (9)0.0231 (7)0.0271 (8)0.0038 (6)0.0015 (6)0.0011 (6)
C90.0445 (10)0.0240 (8)0.0308 (8)0.0027 (7)0.0020 (7)0.0056 (6)
C100.0390 (9)0.0283 (8)0.0220 (8)0.0006 (7)0.0001 (6)0.0041 (6)
C110.0258 (7)0.0255 (7)0.0212 (7)0.0001 (6)0.0022 (5)0.0002 (6)
C120.0281 (7)0.0277 (7)0.0184 (7)0.0001 (6)0.0005 (5)0.0013 (5)
C130.0383 (9)0.0246 (7)0.0261 (8)0.0045 (6)0.0014 (6)0.0044 (6)
C140.0447 (9)0.0225 (7)0.0249 (8)0.0060 (7)0.0026 (7)0.0016 (6)
C150.0271 (7)0.0262 (7)0.0206 (7)0.0033 (6)0.0016 (5)0.0021 (5)
C160.0246 (7)0.0234 (7)0.0205 (7)0.0018 (5)0.0019 (5)0.0010 (5)
O10.0498 (8)0.0353 (7)0.0382 (7)0.0066 (6)0.0060 (6)0.0056 (6)
Geometric parameters (Å, º) top
Ni1—O22.0601 (14)O1—H10.74 (3)
Ni1—O32.0945 (14)O1—H1'0.73 (3)
Ni1—O42.0852 (13)N7—C81.320 (2)
Ni1—O52.0585 (12)N7—C161.365 (2)
Ni1—O62.0209 (12)C8—C91.407 (2)
Ni1—N72.0658 (14)C9—C101.362 (2)
S17—O181.4655 (13)C10—C111.423 (2)
S17—O191.4622 (13)C11—C121.423 (2)
S17—O201.4472 (13)C11—C161.417 (2)
S17—C121.7601 (16)C12—C131.379 (2)
O6—C151.3211 (19)C13—C141.402 (2)
O2—H20.81 (2)C14—C151.383 (2)
O2—H2'0.79 (3)C15—C161.442 (2)
O3—H3'0.76 (3)C8—H80.964 (18)
O3—H30.82 (3)C9—H90.953 (19)
O4—H4'0.82 (3)C10—H100.97 (2)
O4—H40.78 (3)C13—H130.970 (18)
O5—H50.83 (2)C14—H140.937 (19)
O5—H5'0.87 (3)
O2—Ni1—O388.00 (6)Ni1—O5—H5117.1 (16)
O2—Ni1—O487.28 (6)H1—O1—H1'108 (3)
O2—Ni1—O589.28 (5)C8—N7—C16119.21 (14)
O2—Ni1—O6175.96 (5)Ni1—N7—C16110.67 (10)
O2—Ni1—N797.35 (5)Ni1—N7—C8130.12 (11)
O3—Ni1—O4175.02 (6)N7—C8—C9122.12 (15)
O3—Ni1—O588.91 (6)C8—C9—C10119.93 (15)
O3—Ni1—O688.05 (5)C9—C10—C11119.71 (14)
O3—Ni1—N791.94 (6)C10—C11—C12125.38 (14)
O4—Ni1—O589.44 (5)C12—C11—C16118.02 (13)
O4—Ni1—O696.69 (5)C10—C11—C16116.60 (13)
O4—Ni1—N790.24 (5)S17—C12—C13119.23 (12)
O5—Ni1—O691.50 (5)S17—C12—C11121.13 (11)
O5—Ni1—N7173.34 (5)C11—C12—C13119.64 (14)
O6—Ni1—N781.93 (5)C12—C13—C14122.08 (15)
O18—S17—O19111.65 (7)C13—C14—C15120.90 (14)
O18—S17—O20112.27 (7)C14—C15—C16117.57 (14)
O18—S17—C12105.33 (7)O6—C15—C14123.42 (14)
O19—S17—O20112.20 (7)O6—C15—C16119.01 (13)
O19—S17—C12106.87 (7)N7—C16—C15115.85 (13)
O20—S17—C12108.05 (7)N7—C16—C11122.42 (13)
Ni1—O6—C15111.94 (9)C11—C16—C15121.72 (13)
H2—O2—H2'104 (3)C9—C8—H8120.8 (10)
Ni1—O2—H2121.9 (19)N7—C8—H8117.1 (10)
Ni1—O2—H2'122 (2)C8—C9—H9121.1 (13)
Ni1—O3—H3115 (2)C10—C9—H9118.9 (13)
Ni1—O3—H3'109 (2)C11—C10—H10120.1 (11)
H3—O3—H3'109 (3)C9—C10—H10120.1 (11)
Ni1—O4—H4113 (2)C12—C13—H13119.2 (11)
H4—O4—H4'111 (3)C14—C13—H13118.7 (11)
Ni1—O4—H4'109.4 (17)C13—C14—H14122.2 (13)
Ni1—O5—H5'116.4 (18)C15—C14—H14116.9 (13)
H5—O5—H5'107 (2)
O3—Ni1—O6—C1585.26 (10)Ni1—N7—C16—C153.17 (16)
O4—Ni1—O6—C1596.27 (10)C16—N7—C8—C90.8 (2)
O5—Ni1—O6—C15174.12 (10)N7—C8—C9—C100.5 (3)
N7—Ni1—O6—C156.98 (10)C8—C9—C10—C110.8 (3)
O2—Ni1—N7—C88.99 (14)C9—C10—C11—C12180.00 (16)
O2—Ni1—N7—C16170.54 (10)C9—C10—C11—C160.0 (2)
O3—Ni1—N7—C897.22 (14)C10—C11—C12—S170.2 (2)
O3—Ni1—N7—C1682.31 (10)C12—C11—C16—C152.4 (2)
O4—Ni1—N7—C878.30 (14)C10—C11—C12—C13179.61 (15)
O4—Ni1—N7—C16102.17 (10)C10—C11—C16—C15177.59 (14)
O6—Ni1—N7—C8175.03 (14)C12—C11—C16—N7178.73 (14)
O6—Ni1—N7—C165.44 (10)C16—C11—C12—C130.4 (2)
O18—S17—C12—C134.49 (14)C10—C11—C16—N71.3 (2)
O19—S17—C12—C13123.37 (13)C16—C11—C12—S17179.77 (11)
O20—S17—C12—C13115.69 (13)S17—C12—C13—C14178.83 (12)
O20—S17—C12—C1163.70 (14)C11—C12—C13—C140.6 (2)
O18—S17—C12—C11176.12 (12)C12—C13—C14—C150.5 (2)
O19—S17—C12—C1157.25 (14)C13—C14—C15—C162.4 (2)
Ni1—O6—C15—C14173.08 (12)C13—C14—C15—O6177.01 (14)
Ni1—O6—C15—C167.50 (17)O6—C15—C16—N72.9 (2)
Ni1—N7—C16—C11177.90 (11)O6—C15—C16—C11176.04 (13)
Ni1—N7—C8—C9178.69 (13)C14—C15—C16—N7177.65 (13)
C8—N7—C16—C111.7 (2)C14—C15—C16—C113.4 (2)
C8—N7—C16—C15177.24 (13)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1—H1···O190.74 (3)2.12 (3)2.824 (2)159 (3)
O1—H1···O6i0.73 (3)2.12 (3)2.830 (2)165 (3)
O2—H2···O19i0.81 (2)1.96 (3)2.7644 (19)170 (2)
O2—H2···O4ii0.79 (3)2.11 (3)2.879 (2)166 (3)
O3—H3···O18i0.82 (3)1.98 (3)2.7756 (19)165 (3)
O3—H3···O1iii0.76 (3)2.16 (3)2.900 (2)162 (3)
O4—H4···O1iv0.78 (3)1.93 (3)2.690 (2)166 (3)
O4—H4···O18v0.82 (3)1.93 (2)2.7133 (18)161 (2)
O5—H5···O6vi0.83 (2)1.94 (2)2.7677 (18)172 (2)
O5—H5···O20iii0.87 (3)1.94 (3)2.8075 (18)169 (2)
C8—H8···O19i0.964 (18)2.534 (16)3.267 (2)132.8 (12)
C13—H13···O180.970 (18)2.399 (19)2.831 (2)106.4 (13)
C14—H14···O20vii0.937 (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) x1/2, y+1/2, z+1/2; (v) x1/2, y+1/2, z+1/2; (vi) x, y, z+1; (vii) x1/2, y1/2, z+1/2.
 

Subscribe to Acta Crystallographica Section E: Crystallographic Communications

The full text of this article is available to subscribers to the journal.

If you have already registered and are using a computer listed in your registration details, please email support@iucr.org for assistance.

Buy online

You may purchase this article in PDF and/or HTML formats. For purchasers in the European Community who do not have a VAT number, VAT will be added at the local rate. Payments to the IUCr are handled by WorldPay, who will accept payment by credit card in several currencies. To purchase the article, please complete the form below (fields marked * are required), and then click on `Continue'.
E-mail address* 
Repeat e-mail address* 
(for error checking) 

Format*   PDF (US $40)
   HTML (US $40)
   PDF+HTML (US $50)
In order for VAT to be shown for your country javascript needs to be enabled.

VAT number 
(non-UK EC countries only) 
Country* 
 

Terms and conditions of use
Contact us

Follow Acta Cryst. E
Sign up for e-alerts
Follow Acta Cryst. on Twitter
Follow us on facebook
Sign up for RSS feeds