Tetra­aqua(8-hydroxy­quinoline-5-sulfo­nato-N,O)­nickel(II) monohydrate

In the title compound, [Ni(HQS)(H₂O)₄]·H₂O (HQS is the 8-hydroxy­quinoline-5-sulfonic acid dianion, C₉H₁₃NO₈S), 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.

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


 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

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'

Crystal data

[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) Å^3	0.36 × 0.29 × 0.25 mm
Z = 4

Data collection

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

Refinement on F^2	0 restraints
Least-squares matrix: full	All H-atom parameters refined
R[F^2 > 2σ(F^2)] = 0.023	w = 1/[σ^2(Fo^2) + (0.0377P)^2 + 0.402P] where P = (Fo^2 + 2Fc^2)/3
wR(F^2) = 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

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 (Ų)

	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 (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
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)

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)

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′···O6^i	0.73 (3)	2.12 (3)	2.830 (2)	165 (3)
O2—H2···O19^i	0.81 (2)	1.96 (3)	2.7644 (19)	170 (2)
O2—H2′···O4^ii	0.79 (3)	2.11 (3)	2.879 (2)	166 (3)
O3—H3···O18^i	0.82 (3)	1.98 (3)	2.7756 (19)	165 (3)
O3—H3′···O1^iii	0.76 (3)	2.16 (3)	2.900 (2)	162 (3)
O4—H4···O1^iv	0.78 (3)	1.93 (3)	2.690 (2)	166 (3)
O4—H4′···O18^v	0.82 (3)	1.93 (2)	2.7133 (18)	161 (2)
O5—H5···O6^vi	0.83 (2)	1.94 (2)	2.7677 (18)	172 (2)
O5—H5′···O20^iii	0.87 (3)	1.94 (3)	2.8075 (18)	169 (2)
C8—H8···O19^i	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···O20^vii	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.