Poly[[[diaqua­nickel(II)]-bis­(μ₂-4-aminobenzene­sulfonato] dihydrate]

In the title compound, {[Ni(C₆H₆NO₃S)₂(H₂O)₂]·2H₂O}_n, each Ni^II atom lies on a centre of inversion and is six-coordinated by two N atoms, two sulfonate O atoms and two water mol­ecules in a distorted octa­hedral geometry. The sulfanilate anion, a bidentate bridging ligand, links the Ni^II atoms to produce a layered structure.

Key indicators

• Single-crystal X-ray study
• T = 293 K
• Mean [sigma](C-C) = 0.004 Å
• R factor = 0.031
• wR factor = 0.084
• Data-to-parameter ratio = 11.6

checkCIF/PLATON results

No syntax errors found



Alert level C
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ ....          ?
PLAT417_ALERT_2_C Short Inter D-H..H-D       H21    ..  H32     ..       2.12 Ang.

Alert level G
PLAT199_ALERT_1_G Check the Reported _cell_measurement_temperature        293 K
PLAT200_ALERT_1_G Check the Reported _diffrn_ambient_temperature .        293 K

   0 ALERT level A = In general: serious problem
   0 ALERT level B = Potentially serious problem
   2 ALERT level C = Check and explain
   2 ALERT level G = General alerts; check

   3 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
   1 ALERT type 2 Indicator that the structure model may be wrong or deficient
   0 ALERT type 3 Indicator that the structure quality may be low
   0 ALERT type 4 Improvement, methodology, query or suggestion
   0 ALERT type 5 Informative message, check

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Computing details

Data collection: SMART (Bruker, 1998); cell refinement: SAINT (Bruker, 1998); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL-Plus (Sheldrick, 1990); software used to prepare material for publication: SHELXTL-Plus.

Poly[[[diaquanickel(II)]-bis(µ₂-4-aminobenzenesulfonato] dihydrate]

Crystal data

[Ni(C6H6NO3S)2(H2O)2]·2H2O	F(000) = 492
Mr = 475.13	Dx = 1.788 Mg m^−3
Monoclinic, P21/n	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2yn	Cell parameters from 4836 reflections
a = 7.4363 (13) Å	θ = 2.3–26.0°
b = 17.357 (3) Å	µ = 1.39 mm^−1
c = 7.6562 (14) Å	T = 293 K
β = 116.726 (3)°	Block, green
V = 882.6 (3) Å^3	0.27 × 0.21 × 0.19 mm
Z = 2

Data collection

Bruker SMART CCD area-detector diffractometer	1721 independent reflections
Radiation source: fine-focus sealed tube	1497 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.064
Detector resolution: 9.00cm pixels mm^-1	θmax = 26.0°, θmin = 2.4°
φ and ω scans	h = −5→9
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	k = −21→21
Tmin = 0.718, Tmax = 0.769	l = −9→9
4836 measured reflections

Refinement

Refinement on F^2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.031	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.084	H atoms treated by a mixture of independent and constrained refinement
S = 1.01	w = 1/[σ^2(Fo^2) + (0.0488P)^2] where P = (Fo^2 + 2Fc^2)/3
1721 reflections	(Δ/σ)max = 0.001
148 parameters	Δρmax = 0.54 e Å^−3
6 restraints	Δρmin = −0.40 e Å^−3

Special details

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 (Ų)

	x	y	z	Uiso*/Ueq
Ni1	0.5000	1.0000	0.0000	0.01931 (15)
C1	0.7871 (3)	0.69889 (13)	0.0885 (3)	0.0233 (5)
C2	0.9090 (4)	0.75749 (13)	0.0816 (4)	0.0276 (5)
H2	1.0146	0.7467	0.0517	0.033*
C3	0.8733 (4)	0.83269 (13)	0.1193 (3)	0.0274 (5)
H3	0.9541	0.8725	0.1133	0.033*
C4	0.7174 (3)	0.84851 (12)	0.1660 (3)	0.0232 (5)
C5	0.5915 (4)	0.78978 (13)	0.1674 (4)	0.0300 (6)
H5	0.4834	0.8008	0.1933	0.036*
C6	0.6271 (4)	0.71451 (13)	0.1300 (4)	0.0303 (6)
H6	0.5444	0.6748	0.1327	0.036*
N1	0.6858 (3)	0.92637 (11)	0.2142 (3)	0.0251 (4)
O1	0.8983 (3)	0.60272 (9)	−0.1047 (2)	0.0326 (4)
O2	0.6574 (2)	0.55804 (9)	0.0080 (2)	0.0305 (4)
O3	1.0067 (2)	0.57714 (9)	0.2389 (2)	0.0289 (4)
O1W	0.7297 (3)	1.05618 (11)	−0.0085 (3)	0.0371 (4)
O2W	0.3909 (3)	0.56720 (14)	0.2413 (3)	0.0476 (5)
S1	0.84058 (9)	0.60234 (3)	0.05456 (8)	0.02228 (17)
H32	0.379 (6)	0.5287 (17)	0.166 (5)	0.079 (12)*
H31	0.312 (8)	0.559 (4)	0.291 (8)	0.19 (3)*
H12	0.637 (4)	0.9253 (15)	0.293 (3)	0.035 (8)*
H11	0.801 (3)	0.9496 (15)	0.272 (3)	0.036 (8)*
H21	0.856 (3)	1.0597 (18)	0.081 (4)	0.052 (9)*
H22	0.719 (6)	1.055 (2)	−0.123 (3)	0.093 (14)*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Ni1	0.0223 (2)	0.0158 (2)	0.0218 (2)	0.00058 (15)	0.01167 (19)	0.00147 (15)
C1	0.0295 (12)	0.0198 (11)	0.0212 (11)	0.0020 (9)	0.0118 (10)	−0.0006 (9)
C2	0.0300 (13)	0.0250 (12)	0.0336 (13)	0.0002 (10)	0.0195 (11)	−0.0022 (10)
C3	0.0312 (13)	0.0225 (12)	0.0308 (12)	−0.0038 (10)	0.0161 (11)	0.0001 (10)
C4	0.0297 (12)	0.0187 (11)	0.0199 (10)	0.0033 (9)	0.0098 (10)	0.0013 (9)
C5	0.0330 (14)	0.0246 (13)	0.0406 (14)	0.0023 (10)	0.0240 (12)	−0.0001 (10)
C6	0.0368 (14)	0.0217 (12)	0.0385 (13)	−0.0027 (10)	0.0223 (12)	−0.0009 (10)
N1	0.0313 (12)	0.0208 (10)	0.0242 (10)	−0.0001 (9)	0.0133 (10)	−0.0023 (8)
O1	0.0474 (11)	0.0307 (10)	0.0297 (9)	0.0011 (8)	0.0263 (9)	−0.0016 (7)
O2	0.0329 (10)	0.0218 (9)	0.0370 (10)	−0.0017 (7)	0.0159 (8)	−0.0023 (7)
O3	0.0304 (9)	0.0277 (9)	0.0285 (8)	0.0035 (7)	0.0131 (8)	0.0036 (7)
O1W	0.0328 (11)	0.0512 (12)	0.0280 (10)	−0.0111 (9)	0.0143 (9)	0.0023 (8)
O2W	0.0337 (11)	0.0635 (14)	0.0470 (12)	−0.0071 (9)	0.0195 (10)	−0.0197 (11)
S1	0.0289 (3)	0.0180 (3)	0.0231 (3)	0.0010 (2)	0.0146 (3)	−0.0003 (2)

Geometric parameters (Å, º)

Ni1—O1W^i	1.9934 (18)	C4—N1	1.448 (3)
Ni1—O1W	1.9934 (18)	C5—C6	1.388 (3)
Ni1—N1	2.048 (2)	C5—H5	0.93
Ni1—N1^i	2.048 (2)	C6—H6	0.93
Ni1—O3^ii	2.4251 (15)	N1—H12	0.833 (17)
Ni1—O3^iii	2.4251 (15)	N1—H11	0.869 (17)
C1—C2	1.380 (3)	O1—S1	1.4635 (17)
C1—C6	1.389 (3)	O2—S1	1.4620 (17)
C1—S1	1.769 (2)	O3—S1	1.4632 (17)
C2—C3	1.388 (3)	O1W—H21	0.882 (18)
C2—H2	0.93	O1W—H22	0.845 (19)
C3—C4	1.386 (3)	O2W—H32	0.862 (18)
C3—H3	0.93	O2W—H31	0.84 (6)
C4—C5	1.387 (3)
O1W^i—Ni1—O1W	180	C6—C5—H5	120.1
O1W^i—Ni1—N1	87.03 (8)	C5—C6—C1	119.5 (2)
O1W—Ni1—N1	92.97 (8)	C5—C6—H6	120.2
O1W^i—Ni1—N1^i	92.97 (8)	C1—C6—H6	120.2
O1W—Ni1—N1^i	87.03 (8)	C4—N1—Ni1	120.47 (14)
N1—Ni1—N1^i	180	C4—N1—H12	109.8 (18)
C2—C1—C6	120.7 (2)	Ni1—N1—H12	103.7 (19)
C2—C1—S1	119.84 (18)	C4—N1—H11	109.1 (18)
C6—C1—S1	119.41 (18)	Ni1—N1—H11	105.9 (18)
C1—C2—C3	119.7 (2)	H12—N1—H11	107 (2)
C1—C2—H2	120.2	Ni1—O1W—H21	130 (2)
C3—C2—H2	120.2	Ni1—O1W—H22	110 (3)
C4—C3—C2	120.0 (2)	H21—O1W—H22	112 (3)
C4—C3—H3	120.0	H32—O2W—H31	107 (5)
C2—C3—H3	120.0	O2—S1—O3	111.60 (10)
C3—C4—C5	120.1 (2)	O2—S1—O1	112.93 (10)
C3—C4—N1	120.1 (2)	O3—S1—O1	111.58 (10)
C5—C4—N1	119.8 (2)	O2—S1—C1	106.71 (10)
C4—C5—C6	119.9 (2)	O3—S1—C1	106.84 (10)
C4—C5—H5	120.1	O1—S1—C1	106.73 (10)
C6—C1—C2—C3	1.0 (4)	C3—C4—N1—Ni1	90.3 (2)
S1—C1—C2—C3	−176.34 (18)	C5—C4—N1—Ni1	−89.8 (2)
C1—C2—C3—C4	0.8 (3)	O1W^i—Ni1—N1—C4	77.75 (18)
C2—C3—C4—C5	−2.6 (3)	O1W—Ni1—N1—C4	−102.25 (18)
C2—C3—C4—N1	177.2 (2)	C2—C1—S1—O2	−162.40 (18)
C3—C4—C5—C6	2.7 (4)	C6—C1—S1—O2	20.2 (2)
N1—C4—C5—C6	−177.1 (2)	C2—C1—S1—O3	78.1 (2)
C4—C5—C6—C1	−1.0 (4)	C6—C1—S1—O3	−99.27 (19)
C2—C1—C6—C5	−0.9 (4)	C2—C1—S1—O1	−41.4 (2)
S1—C1—C6—C5	176.46 (18)	C6—C1—S1—O1	141.24 (19)

Symmetry codes: (i) −x+1, −y+2, −z; (ii) x−1/2, −y+3/2, z−1/2; (iii) −x+3/2, y+1/2, −z+1/2.

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
N1—H11···O2^iii	0.87 (2)	2.45 (2)	2.979 (3)	120 (2)
N1—H11···O2^iv	0.87 (2)	2.45 (2)	3.215 (3)	148 (2)
N1—H12···O1^v	0.83 (2)	2.29 (3)	3.068 (3)	156 (2)
O1W—H21···O2W^iii	0.88 (2)	1.76 (3)	2.644 (3)	180 (4)
O1W—H22···O1^vi	0.85 (2)	2.04 (2)	2.792 (3)	148 (4)
O2W—H31···O3^vii	0.84 (6)	2.14 (7)	2.854 (3)	142 (5)
O2W—H32···O2^viii	0.86 (2)	1.95 (3)	2.807 (3)	178 (5)

Symmetry codes: (iii) −x+3/2, y+1/2, −z+1/2; (iv) x+1/2, −y+3/2, z+1/2; (v) x−1/2, −y+3/2, z+1/2; (vi) −x+3/2, y+1/2, −z−1/2; (vii) x−1, y, z; (viii) −x+1, −y+1, −z.