In the title compound, {[Ni(C7H4O5S)(C12H10N2)(H2O)2]·0.25H2O}n, the NiII 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 NiII atoms through one carboxylate O atom and one sulfonate O atom.
Supporting information
CCDC reference: 269546
Key indicators
- Single-crystal X-ray study
- T = 298 K
- Mean (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
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]
top
Crystal data top
[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) Å3 | 0.35 × 0.27 × 0.23 mm |
Z = 8 | |
Data collection top
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 top
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.032 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.083 | H-atom parameters constrained |
S = 1.03 | w = 1/[σ2(Fo2) + (0.0432P)2 + 5.4805P] where P = (Fo2 + 2Fc2)/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 top
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 (Å2) top | 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 (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
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) top
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—C13i | 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—C19ii | 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 | C13i—C13—C10 | 126.1 (3) |
Ni1—O7—H7A | 109.5 | C13i—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) | C19ii—C19—C16 | 125.7 (2) |
C5—C4—C3 | 120.3 (2) | C19ii—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) top
D—H···A | D—H | H···A | D···A | D—H···A |
O7—H7B···O1iii | 0.81 | 2.02 | 2.8273 (18) | 173 |
O7—H7A···O2iv | 0.82 | 1.90 | 2.720 (2) | 175 |
O6—H6B···O2iv | 0.81 | 2.03 | 2.827 (2) | 168 |
O6—H6A···O5v | 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. |