The Ni atom in the zwitterionic title compound, [Ni(C7H6NO2S)2(H2O)4], lies on a centre of symmetry. It is linked to the pyridyl N atom of two anionic groups and to four water molecules in an octahedral environment. The zwitterions are connected by hydrogen bonds into a three-dimensional network structure.
Supporting information
CCDC reference: 234784
Key indicators
- Single-crystal X-ray study
- T = 298 K
- Mean (C-C) = 0.002 Å
- R factor = 0.026
- wR factor = 0.072
- Data-to-parameter ratio = 12.0
checkCIF/PLATON results
No syntax errors found
Alert level C
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ?
PLAT094_ALERT_2_C Ratio of Maximum / Minimum Residual Density .... 2.18
PLAT128_ALERT_4_C Non-standard setting of Space group P21/c .... P21/a
PLAT164_ALERT_4_C Nr. of Refined C-H H-Atoms in Heavy-At Struct... 6
PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 4
0 ALERT level A = In general: serious problem
0 ALERT level B = Potentially serious problem
5 ALERT level C = Check and explain
0 ALERT level G = General alerts; check
1 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
3 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: SMART (Bruker, 2001); cell refinement: SMART; data reduction: SAINT (Bruker, 2001); program(s) used to solve structure: difference Fourier, with Ni at (1/2, 1/2, 1/2); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEPII (Johnson, 1976); software used to prepare material for publication: SHELXL97.
Tetraaquabis(4-pyridylthioactetato)nickel(II)
top
Crystal data top
[Ni(C7H6NO2S)2(H2O)4] | F(000) = 484 |
Mr = 467.15 | Dx = 1.709 Mg m−3 |
Monoclinic, P21/a | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2yab | Cell parameters from 3212 reflections |
a = 7.4924 (5) Å | θ = 2.6–26.9° |
b = 10.4589 (7) Å | µ = 1.35 mm−1 |
c = 12.1369 (8) Å | T = 298 K |
β = 107.393 (1)° | Plate, blue |
V = 907.6 (1) Å3 | 0.35 × 0.19 × 0.09 mm |
Z = 2 | |
Data collection top
Bruker SMART APEX area-detector diffractometer | 1960 independent reflections |
Radiation source: fine-focus sealed tube | 1813 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.015 |
φ and ω scans | θmax = 27.0°, θmin = 1.8° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −8→9 |
Tmin = 0.753, Tmax = 0.889 | k = −13→11 |
5157 measured reflections | l = −15→15 |
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)] = 0.026 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.072 | All H-atom parameters refined |
S = 1.04 | w = 1/[σ2(Fo2) + (0.0462P)2 + 0.1843P] where P = (Fo2 + 2Fc2)/3 |
1960 reflections | (Δ/σ)max = 0.001 |
164 parameters | Δρmax = 0.37 e Å−3 |
10 restraints | Δρmin = −0.17 e Å−3 |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Ni1 | 0.5000 | 0.5000 | 0.5000 | 0.0207 (1) | |
S1 | 0.91703 (6) | 0.69526 (4) | 1.03479 (3) | 0.0314 (1) | |
O1 | 1.0723 (2) | 0.69551 (12) | 1.2810 (1) | 0.0382 (3) | |
O2 | 0.9398 (2) | 0.51701 (14) | 1.3212 (1) | 0.0418 (3) | |
O1w | 0.5797 (2) | 0.31611 (11) | 0.5572 (1) | 0.0301 (3) | |
O2w | 0.7633 (2) | 0.53151 (15) | 0.4890 (1) | 0.0387 (3) | |
N1 | 0.5955 (2) | 0.57068 (12) | 0.6700 (1) | 0.0251 (3) | |
C1 | 0.9667 (2) | 0.60111 (16) | 1.2541 (1) | 0.0297 (3) | |
C2 | 0.8545 (2) | 0.58104 (17) | 1.1281 (1) | 0.0313 (4) | |
C3 | 0.6892 (2) | 0.68180 (16) | 0.6934 (1) | 0.0316 (4) | |
C4 | 0.7813 (2) | 0.72242 (16) | 0.8036 (1) | 0.0307 (3) | |
C5 | 0.7802 (2) | 0.64573 (15) | 0.8975 (1) | 0.0236 (3) | |
C6 | 0.6759 (2) | 0.53384 (16) | 0.8742 (1) | 0.0264 (3) | |
C7 | 0.5875 (2) | 0.50083 (14) | 0.7607 (1) | 0.0263 (3) | |
H1w1 | 0.691 (2) | 0.318 (3) | 0.600 (2) | 0.065 (8)* | |
H1w2 | 0.517 (3) | 0.277 (2) | 0.594 (2) | 0.061 (7)* | |
H2w1 | 0.801 (3) | 0.526 (2) | 0.431 (2) | 0.048 (7)* | |
H2w2 | 0.852 (3) | 0.515 (2) | 0.548 (2) | 0.056 (8)* | |
H2a | 0.725 (2) | 0.589 (2) | 1.121 (2) | 0.042 (6)* | |
H2b | 0.878 (4) | 0.495 (1) | 1.110 (2) | 0.053 (7)* | |
H3 | 0.698 (3) | 0.731 (2) | 0.630 (1) | 0.046 (6)* | |
H4 | 0.845 (2) | 0.802 (1) | 0.814 (2) | 0.036 (5)* | |
H6 | 0.669 (3) | 0.475 (2) | 0.932 (1) | 0.035 (5)* | |
H7 | 0.525 (2) | 0.421 (1) | 0.747 (2) | 0.027 (4)* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Ni1 | 0.0223 (2) | 0.0242 (2) | 0.0147 (2) | −0.0004 (1) | 0.0041 (1) | 0.0010 (1) |
S1 | 0.0354 (2) | 0.0352 (2) | 0.0196 (2) | −0.0083 (2) | 0.0021 (2) | −0.0036 (2) |
O1 | 0.0402 (7) | 0.0397 (7) | 0.0268 (6) | 0.0042 (5) | −0.0021 (5) | −0.0075 (5) |
O2 | 0.0422 (8) | 0.0611 (9) | 0.0216 (6) | 0.0018 (6) | 0.0086 (5) | 0.0050 (5) |
O1w | 0.0353 (7) | 0.0279 (6) | 0.0241 (6) | 0.0027 (5) | 0.0044 (5) | 0.0042 (4) |
O2w | 0.0258 (6) | 0.0661 (8) | 0.0243 (6) | −0.0024 (6) | 0.0080 (5) | 0.0051 (6) |
N1 | 0.0287 (6) | 0.0276 (7) | 0.0174 (6) | −0.0006 (5) | 0.0045 (5) | 0.0002 (5) |
C1 | 0.0280 (8) | 0.0414 (9) | 0.0183 (7) | 0.0102 (7) | 0.0046 (6) | −0.0038 (6) |
C2 | 0.0324 (8) | 0.0397 (9) | 0.0196 (7) | −0.0015 (7) | 0.0045 (6) | −0.0002 (6) |
C3 | 0.0409 (9) | 0.0306 (8) | 0.0217 (8) | −0.0060 (7) | 0.0070 (7) | 0.0034 (6) |
C4 | 0.0381 (9) | 0.0279 (8) | 0.0249 (8) | −0.0084 (7) | 0.0077 (7) | −0.0003 (6) |
C5 | 0.0229 (7) | 0.0281 (8) | 0.0180 (7) | 0.0009 (6) | 0.0036 (5) | −0.0022 (6) |
C6 | 0.0333 (8) | 0.0259 (7) | 0.0191 (7) | −0.0010 (6) | 0.0067 (6) | 0.0015 (6) |
C7 | 0.0310 (9) | 0.0263 (8) | 0.0203 (8) | −0.0039 (6) | 0.0057 (6) | −0.0018 (5) |
Geometric parameters (Å, º) top
Ni1—O1w | 2.071 (1) | C4—C5 | 1.395 (2) |
Ni1—O1wi | 2.071 (1) | C5—C6 | 1.389 (2) |
Ni1—O2w | 2.044 (1) | C6—C7 | 1.382 (2) |
Ni1—O2wi | 2.044 (1) | O1w—H1w1 | 0.84 (1) |
Ni1—N1 | 2.106 (1) | O1w—H1w2 | 0.84 (1) |
Ni1—N1i | 2.106 (1) | O2w—H2w1 | 0.83 (1) |
S1—C2 | 1.802 (2) | O2w—H2w2 | 0.84 (1) |
S1—C5 | 1.754 (2) | C2—H2a | 0.95 (1) |
O1—C1 | 1.246 (2) | C2—H2b | 0.95 (1) |
O2—C1 | 1.255 (2) | C3—H3 | 0.95 (1) |
N1—C7 | 1.337 (2) | C4—H4 | 0.95 (1) |
N1—C3 | 1.344 (2) | C6—H6 | 0.95 (1) |
C1—C2 | 1.523 (2) | C7—H7 | 0.95 (1) |
C3—C4 | 1.376 (2) | | |
| | | |
O1w—Ni1—O1wi | 180 | C6—C5—C4 | 117.3 (1) |
O1w—Ni1—O2w | 89.1 (1) | C6—C5—S1 | 125.1 (1) |
O1w—Ni1—O2wi | 90.9 (1) | C4—C5—S1 | 117.5 (1) |
O1w—Ni1—N1 | 91.0 (1) | C7—C6—C5 | 119.1 (1) |
O1w—Ni1—N1i | 89.0 (1) | N1—C7—C6 | 123.9 (1) |
O1wi—Ni1—O2w | 90.9 (1) | Ni1—O1w—H1w1 | 109 (2) |
O1wi—Ni1—O2wi | 89.1 (1) | Ni1—O1w—H1w2 | 118 (2) |
O1wi—Ni1—N1 | 89.0 (1) | H1w1—O1w—H1w2 | 107 (2) |
O1wi—Ni1—N1i | 91.0 (1) | Ni1—O2w—H2w1 | 129 (2) |
O2w—Ni1—O2wi | 180 | Ni1—O2w—H2w2 | 117 (2) |
O2w—Ni1—N1 | 87.5 (1) | H2w1—O2w—H2w2 | 109 (3) |
O2w—Ni1—N1i | 92.5 (1) | C1—C2—H2a | 109 (1) |
O2wi—Ni1—N1 | 92.5 (1) | S1—C2—H2a | 110 (1) |
O2wi—Ni1—N1i | 87.5 (1) | C1—C2—H2b | 106 (2) |
N1—Ni1—N1i | 180 | S1—C2—H2b | 113 (2) |
C5—S1—C2 | 102.3 (1) | H2a—C2—H2b | 108 (2) |
C7—N1—C3 | 116.6 (1) | N1—C3—H3 | 117 (1) |
C7—N1—Ni1 | 122.0 (1) | C4—C3—H3 | 119 (1) |
C3—N1—Ni1 | 120.9 (1) | C3—C4—H4 | 119 (1) |
O1—C1—O2 | 126.7 (2) | C5—C4—H4 | 122 (1) |
O1—C1—C2 | 119.3 (2) | C7—C6—H6 | 118 (1) |
O2—C1—C2 | 114.0 (2) | C5—C6—H6 | 123 (1) |
C1—C2—S1 | 111.7 (1) | N1—C7—H7 | 118 (1) |
N1—C3—C4 | 123.4 (1) | C6—C7—H7 | 118 (1) |
C3—C4—C5 | 119.5 (2) | | |
| | | |
O2w—Ni1—N1—C7 | −121.8 (1) | Ni1—N1—C3—C4 | −168.9 (1) |
O2wi—Ni1—N1—C7 | 58.2 (1) | N1—C3—C4—C5 | 0.4 (3) |
O1w—Ni1—N1—C7 | −32.7 (1) | C3—C4—C5—C6 | −3.4 (2) |
O1wi—Ni1—N1—C7 | 147.3 (1) | C3—C4—C5—S1 | 174.4 (1) |
O2w—Ni1—N1—C3 | 49.5 (1) | C2—S1—C5—C6 | −8.4 (2) |
O2wi—Ni1—N1—C3 | −130.5 (1) | C2—S1—C5—C4 | 174.0 (1) |
O1w—Ni1—N1—C3 | 138.5 (1) | C4—C5—C6—C7 | 3.3 (2) |
O1wi—Ni1—N1—C3 | −41.5 (1) | S1—C5—C6—C7 | −174.3 (1) |
O1—C1—C2—S1 | 6.2 (2) | C3—N1—C7—C6 | −2.9 (2) |
O2—C1—C2—S1 | −174.1 (1) | Ni1—N1—C7—C6 | 168.7 (1) |
C5—S1—C2—C1 | 176.8 (1) | C5—C6—C7—N1 | −0.1 (3) |
C7—N1—C3—C4 | 2.8 (2) | | |
Symmetry code: (i) −x+1, −y+1, −z+1. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O1w—H1w1···O1ii | 0.84 (1) | 1.93 (1) | 2.759 (2) | 168 (3) |
O1w—H1w2···O1iii | 0.84 (1) | 2.02 (1) | 2.842 (2) | 165 (2) |
O2w—H2w1···O2iv | 0.83 (1) | 1.92 (1) | 2.744 (2) | 168 (2) |
O2w—H2w2···O2ii | 0.84 (1) | 1.89 (1) | 2.729 (2) | 177 (3) |
Symmetry codes: (ii) −x+2, −y+1, −z+2; (iii) −x+3/2, y−1/2, −z+2; (iv) x, y, z−1. |