catena-Poly­[[[di­aqua(2-sulfonatobenzoato)­nickel(II)]-μ-1,2-di-4-pyridyl­ethyl­ene] 0.25-hydrate]

In the title compound, {[Ni(C₇H₄O₅S)(C₁₂H₁₀N₂)(H₂O)₂]·0.25H₂O}_n, the Ni^II atom has a distorted octahedral environment formed by two N and four O atoms. The 1,2-di-4-pyridyl­ethyl­ene ligands, which lie on inversion centers, function as μ₂-bridging ligands to form a linear chain. The 2-sulfonatobenzoate ligands protrude alternately on both sides of the linear chain and chelate to the Ni^II atoms through one carboxyl­ate O atom and one sulfonate O atom.

Key indicators

• Single-crystal X-ray study
• T = 298 K
• Mean [sigma](C-C) = 0.003 Å
• H-atom completeness 98%
• Disorder in solvent or counterion
• R factor = 0.032
• wR factor = 0.083
• Data-to-parameter ratio = 15.9

checkCIF/PLATON results

No syntax errors found



Alert level C
PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings    Differ ....          ?
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ ....          ?
PLAT045_ALERT_1_C Calculated and Reported Z Differ by ............       0.12 Ratio
PLAT068_ALERT_1_C Reported F000 Differs from Calcd (or Missing)...          ?
PLAT076_ALERT_1_C Occupancy       0.50 less than 1.0 for Sp.pos  .         O8
PLAT302_ALERT_4_C Anion/Solvent Disorder .........................      50.00 Perc.

Alert level G
FORMU01_ALERT_2_G  There is a discrepancy between the atom counts in the
            _chemical_formula_sum and the formula from the _atom_site* data.
            Atom count from _chemical_formula_sum:C19 H18.5 N2 Ni1 O7.25 S1
            Atom count from the _atom_site data:  C19 H18 N2 Ni1 O7.25 S1
CELLZ01_ALERT_1_G Difference between formula and atom_site contents detected.
CELLZ01_ALERT_1_G WARNING: H atoms missing from atom site list. Is this intentional?
           From the CIF: _cell_formula_units_Z    8
           From the CIF: _chemical_formula_sum  C19 H18.5 N2 Ni1 O7.25 S1
           TEST: Compare cell contents of formula and atom_site data

           atom    Z*formula  cif sites diff
           C        152.00    152.00    0.00
           H        148.00    144.00    4.00
           N         16.00     16.00    0.00
           Ni         8.00      8.00    0.00
           O         58.00     58.00    0.00
           S          8.00      8.00    0.00

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

   7 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
   1 ALERT type 4 Improvement, methodology, query or suggestion

---

Computing details

Data collection: SMART (Bruker, 2002); cell refinement: SAINT (Bruker, 2002); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: XP (Bruker, 2002); software used to prepare material for publication: SHELXTL (Bruker, 2002).

catena-Poly[[[diaqua(2-sulfonatobenzoato)nickel(II)]-µ-1,2-di-4- pyridylethylene] 0.25-hydrate]

Crystal data

[Ni(C7H4O5S)(C12H10N2)(H2O)2]·0.25H2O	F(000) = 1988
Mr = 481.63	Dx = 1.572 Mg m^−3
Monoclinic, C2/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2yc	Cell parameters from 6367 reflections
a = 17.1636 (9) Å	θ = 2.4–28.2°
b = 16.5180 (9) Å	µ = 1.10 mm^−1
c = 14.6151 (8) Å	T = 298 K
β = 100.798 (1)°	Prism, green
V = 4070.1 (4) Å^3	0.35 × 0.27 × 0.23 mm
Z = 8

Data collection

Bruker SMART CCD area-detector diffractometer	4429 independent reflections
Radiation source: fine-focus sealed tube	4072 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.020
φ and ω scans	θmax = 27.0°, θmin = 1.7°
Absorption correction: multi-scan (SADABS; Bruker, 2000)	h = −21→17
Tmin = 0.699, Tmax = 0.786	k = −21→17
12199 measured reflections	l = −18→18

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)] = 0.032	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.083	H-atom parameters constrained
S = 1.03	w = 1/[σ^2(Fo^2) + (0.0432P)^2 + 5.4805P] where P = (Fo^2 + 2Fc^2)/3
4429 reflections	(Δ/σ)max = 0.002
278 parameters	Δρmax = 0.63 e Å^−3
10 restraints	Δρmin = −0.36 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	Occ. (<1)
Ni1	0.884043 (12)	0.897732 (14)	1.008807 (15)	0.01700 (8)
S1	0.80471 (3)	0.79708 (3)	0.82499 (3)	0.02335 (12)
O1	0.90455 (7)	0.95916 (8)	0.89322 (9)	0.0238 (3)
O2	0.89727 (9)	1.02135 (10)	0.75828 (10)	0.0335 (3)
O3	0.86777 (9)	0.79861 (10)	0.77235 (10)	0.0335 (3)
O4	0.83331 (8)	0.80180 (8)	0.92626 (9)	0.0226 (3)
O5	0.75137 (9)	0.72857 (10)	0.80329 (11)	0.0357 (4)
O6	0.87651 (8)	0.84251 (9)	1.13900 (9)	0.0269 (3)
H6A	0.8341	0.8185	1.1343	0.040*
H6B	0.8790	0.8778	1.1783	0.040*
O7	0.93418 (8)	0.99581 (8)	1.08623 (9)	0.0256 (3)
H7A	0.9244	0.9930	1.1390	0.038*
H7B	0.9816	1.0045	1.0938	0.038*
O8	0.5000	0.1761 (3)	0.7500	0.0622 (16)	0.50
N1	0.76944 (9)	0.94160 (10)	1.00886 (11)	0.0219 (3)
N2	0.99479 (9)	0.84325 (10)	1.01727 (11)	0.0218 (3)
C1	0.86680 (11)	0.98053 (11)	0.81413 (13)	0.0232 (4)
C2	0.77953 (12)	0.96185 (13)	0.78776 (13)	0.0267 (4)
C3	0.74586 (12)	0.88496 (13)	0.79180 (14)	0.0268 (4)
C4	0.66425 (13)	0.87498 (17)	0.76669 (17)	0.0414 (6)
H4	0.6421	0.8237	0.7682	0.050*
C5	0.61584 (14)	0.9409 (2)	0.73952 (19)	0.0517 (7)
H5	0.5612	0.9337	0.7234	0.062*
C6	0.64758 (15)	1.01624 (19)	0.73623 (19)	0.0509 (7)
H6	0.6146	1.0605	0.7189	0.061*
C7	0.72931 (14)	1.02695 (16)	0.75879 (16)	0.0392 (5)
H7	0.7507	1.0782	0.7545	0.047*
C8	0.75027 (12)	1.01980 (13)	1.00445 (17)	0.0321 (5)
H8	0.7903	1.0578	1.0043	0.039*
C9	0.67367 (12)	1.04696 (14)	1.00009 (19)	0.0389 (5)
H9	0.6630	1.1022	0.9967	0.047*
C10	0.61229 (11)	0.99224 (14)	1.00076 (15)	0.0306 (5)
C11	0.63270 (12)	0.91089 (13)	1.00691 (16)	0.0296 (4)
H11	0.5940	0.8718	1.0084	0.036*
C12	0.71035 (11)	0.88833 (12)	1.01076 (14)	0.0254 (4)
H12	0.7227	0.8335	1.0149	0.031*
C13	0.53102 (12)	1.02201 (15)	0.99555 (18)	0.0381 (5)
H13	0.5226	1.0771	0.9850	0.046*
C14	1.04473 (11)	0.83554 (13)	1.09886 (14)	0.0278 (4)
H14	1.0273	0.8505	1.1530	0.033*
C15	1.12092 (12)	0.80636 (13)	1.10635 (14)	0.0291 (4)
H15	1.1533	0.8015	1.1647	0.035*
C16	1.14939 (11)	0.78418 (12)	1.02722 (14)	0.0241 (4)
C17	1.09644 (12)	0.79025 (14)	0.94250 (14)	0.0304 (5)
H17	1.1119	0.7744	0.8875	0.037*
C18	1.02115 (11)	0.81987 (13)	0.94077 (14)	0.0282 (4)
H18	0.9869	0.8238	0.8836	0.034*
C19	1.23182 (11)	0.75747 (12)	1.03522 (14)	0.0267 (4)
H19	1.2611	0.7504	1.0950	0.032*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Ni1	0.01229 (12)	0.02105 (13)	0.01804 (13)	0.00121 (8)	0.00387 (8)	0.00066 (8)
S1	0.0210 (2)	0.0279 (2)	0.0210 (2)	−0.00475 (18)	0.00349 (17)	−0.00201 (18)
O1	0.0186 (6)	0.0303 (7)	0.0223 (7)	−0.0017 (5)	0.0035 (5)	0.0061 (5)
O2	0.0369 (8)	0.0391 (9)	0.0265 (7)	−0.0046 (7)	0.0113 (6)	0.0089 (6)
O3	0.0313 (8)	0.0439 (9)	0.0282 (8)	−0.0002 (6)	0.0131 (6)	−0.0029 (6)
O4	0.0227 (6)	0.0238 (7)	0.0206 (6)	−0.0013 (5)	0.0025 (5)	−0.0006 (5)
O5	0.0368 (8)	0.0362 (8)	0.0322 (8)	−0.0145 (7)	0.0015 (6)	−0.0061 (7)
O6	0.0244 (7)	0.0314 (8)	0.0258 (7)	−0.0028 (6)	0.0065 (6)	0.0005 (6)
O7	0.0202 (7)	0.0319 (7)	0.0257 (7)	−0.0055 (5)	0.0064 (5)	−0.0051 (6)
O8	0.055 (3)	0.035 (3)	0.092 (4)	0.000	0.002 (3)	0.000
N1	0.0155 (7)	0.0265 (8)	0.0242 (8)	0.0017 (6)	0.0052 (6)	0.0003 (6)
N2	0.0154 (7)	0.0271 (8)	0.0228 (8)	0.0039 (6)	0.0037 (6)	−0.0006 (6)
C1	0.0237 (9)	0.0235 (9)	0.0234 (9)	0.0003 (7)	0.0068 (7)	0.0025 (7)
C2	0.0245 (10)	0.0361 (11)	0.0191 (9)	0.0035 (8)	0.0029 (7)	0.0067 (8)
C3	0.0205 (9)	0.0392 (11)	0.0200 (9)	0.0006 (8)	0.0021 (7)	0.0039 (8)
C4	0.0239 (11)	0.0586 (16)	0.0396 (13)	−0.0053 (10)	0.0008 (9)	0.0081 (11)
C5	0.0196 (11)	0.083 (2)	0.0504 (15)	0.0077 (12)	0.0019 (10)	0.0161 (14)
C6	0.0356 (13)	0.0681 (19)	0.0477 (15)	0.0251 (13)	0.0042 (11)	0.0162 (13)
C7	0.0371 (12)	0.0437 (13)	0.0358 (12)	0.0103 (10)	0.0041 (10)	0.0112 (10)
C8	0.0208 (10)	0.0248 (10)	0.0528 (13)	−0.0014 (8)	0.0121 (9)	0.0017 (9)
C9	0.0237 (10)	0.0261 (11)	0.0687 (17)	0.0042 (8)	0.0131 (10)	0.0038 (11)
C10	0.0170 (9)	0.0344 (11)	0.0413 (12)	0.0043 (8)	0.0081 (8)	0.0010 (9)
C11	0.0165 (9)	0.0312 (11)	0.0424 (12)	−0.0015 (8)	0.0089 (8)	−0.0003 (9)
C12	0.0196 (9)	0.0259 (10)	0.0321 (10)	0.0010 (7)	0.0080 (8)	0.0002 (8)
C13	0.0205 (10)	0.0349 (12)	0.0599 (15)	0.0085 (9)	0.0098 (10)	0.0025 (10)
C14	0.0210 (9)	0.0405 (12)	0.0220 (9)	0.0073 (8)	0.0039 (7)	−0.0016 (8)
C15	0.0208 (9)	0.0415 (12)	0.0233 (10)	0.0087 (8)	−0.0001 (7)	0.0009 (8)
C16	0.0164 (9)	0.0253 (10)	0.0311 (10)	0.0032 (7)	0.0056 (7)	0.0018 (8)
C17	0.0213 (9)	0.0463 (13)	0.0248 (10)	0.0082 (9)	0.0072 (8)	−0.0034 (9)
C18	0.0196 (9)	0.0424 (12)	0.0221 (10)	0.0082 (8)	0.0022 (7)	−0.0013 (8)
C19	0.0169 (9)	0.0315 (10)	0.0307 (10)	0.0053 (8)	0.0015 (7)	0.0030 (8)

Geometric parameters (Å, º)

Ni1—O1	2.0567 (13)	C5—H5	0.9300
Ni1—O7	2.0690 (13)	C6—C7	1.391 (3)
Ni1—O4	2.0812 (13)	C6—H6	0.9300
Ni1—N2	2.0856 (15)	C7—H7	0.9300
Ni1—N1	2.0963 (15)	C8—C9	1.379 (3)
Ni1—O6	2.1358 (14)	C8—H8	0.9300
S1—O3	1.4409 (15)	C9—C10	1.390 (3)
S1—O5	1.4527 (15)	C9—H9	0.9300
S1—O4	1.4716 (14)	C10—C11	1.387 (3)
S1—C3	1.783 (2)	C10—C13	1.467 (3)
O1—C1	1.265 (2)	C11—C12	1.375 (3)
O2—C1	1.247 (2)	C11—H11	0.9300
O6—H6A	0.8200	C12—H12	0.9300
O6—H6B	0.8134	C13—C13^i	1.316 (5)
O7—H7A	0.8200	C13—H13	0.9300
O7—H7B	0.8133	C14—C15	1.379 (3)
N1—C8	1.332 (3)	C14—H14	0.9300
N1—C12	1.347 (3)	C15—C16	1.387 (3)
N2—C14	1.338 (2)	C15—H15	0.9300
N2—C18	1.339 (2)	C16—C17	1.395 (3)
C1—C2	1.507 (3)	C16—C19	1.466 (2)
C2—C7	1.394 (3)	C17—C18	1.378 (3)
C2—C3	1.401 (3)	C17—H17	0.9300
C3—C4	1.390 (3)	C18—H18	0.9300
C4—C5	1.381 (4)	C19—C19^ii	1.323 (4)
C4—H4	0.9300	C19—H19	0.9300
C5—C6	1.364 (4)
O1—Ni1—O7	86.86 (6)	C3—C4—H4	119.8
O1—Ni1—O4	90.97 (5)	C6—C5—C4	120.4 (2)
O7—Ni1—O4	177.77 (5)	C6—C5—H5	119.8
O1—Ni1—N2	88.13 (6)	C4—C5—H5	119.8
O7—Ni1—N2	91.39 (6)	C5—C6—C7	120.0 (2)
O4—Ni1—N2	89.06 (6)	C5—C6—H6	120.0
O1—Ni1—N1	97.74 (6)	C7—C6—H6	120.0
O7—Ni1—N1	91.34 (6)	C6—C7—C2	120.9 (2)
O4—Ni1—N1	88.43 (6)	C6—C7—H7	119.6
N2—Ni1—N1	173.65 (6)	C2—C7—H7	119.6
O1—Ni1—O6	172.19 (5)	N1—C8—C9	122.86 (19)
O7—Ni1—O6	86.31 (6)	N1—C8—H8	118.6
O4—Ni1—O6	95.89 (5)	C9—C8—H8	118.6
N2—Ni1—O6	88.25 (6)	C8—C9—C10	120.4 (2)
N1—Ni1—O6	86.21 (6)	C8—C9—H9	119.8
O3—S1—O5	113.75 (9)	C10—C9—H9	119.8
O3—S1—O4	113.19 (9)	C11—C10—C9	116.61 (18)
O5—S1—O4	109.79 (8)	C11—C10—C13	123.6 (2)
O3—S1—C3	106.52 (9)	C9—C10—C13	119.8 (2)
O5—S1—C3	105.85 (10)	C12—C11—C10	119.75 (19)
O4—S1—C3	107.20 (9)	C12—C11—H11	120.1
C1—O1—Ni1	138.68 (12)	C10—C11—H11	120.1
S1—O4—Ni1	130.38 (8)	N1—C12—C11	123.37 (19)
Ni1—O6—H6A	109.5	N1—C12—H12	118.3
Ni1—O6—H6B	108.6	C11—C12—H12	118.3
H6A—O6—H6B	109.4	C13^i—C13—C10	126.1 (3)
Ni1—O7—H7A	109.5	C13^i—C13—H13	117.0
Ni1—O7—H7B	121.0	C10—C13—H13	117.0
H7A—O7—H7B	104.9	N2—C14—C15	122.95 (18)
C8—N1—C12	117.04 (16)	N2—C14—H14	118.5
C8—N1—Ni1	123.96 (13)	C15—C14—H14	118.5
C12—N1—Ni1	118.97 (13)	C14—C15—C16	120.23 (18)
C14—N2—C18	117.15 (16)	C14—C15—H15	119.9
C14—N2—Ni1	121.24 (13)	C16—C15—H15	119.9
C18—N2—Ni1	121.44 (12)	C15—C16—C17	116.64 (17)
O2—C1—O1	122.91 (18)	C15—C16—C19	119.92 (18)
O2—C1—C2	117.52 (17)	C17—C16—C19	123.43 (18)
O1—C1—C2	119.41 (16)	C18—C17—C16	119.65 (18)
C7—C2—C3	118.40 (19)	C18—C17—H17	120.2
C7—C2—C1	116.64 (19)	C16—C17—H17	120.2
C3—C2—C1	124.95 (17)	N2—C18—C17	123.34 (18)
C4—C3—C2	120.0 (2)	N2—C18—H18	118.3
C4—C3—S1	117.83 (18)	C17—C18—H18	118.3
C2—C3—S1	122.16 (15)	C19^ii—C19—C16	125.7 (2)
C5—C4—C3	120.3 (2)	C19^ii—C19—H19	117.2
C5—C4—H4	119.8	C16—C19—H19	117.2

Symmetry codes: (i) −x+1, −y+2, −z+2; (ii) −x+5/2, −y+3/2, −z+2.

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
O7—H7B···O1^iii	0.81	2.02	2.8273 (18)	173
O7—H7A···O2^iv	0.82	1.90	2.720 (2)	175
O6—H6B···O2^iv	0.81	2.03	2.827 (2)	168
O6—H6A···O5^v	0.82	2.02	2.757 (2)	149

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