In the linear-chain title compound, [Ni2(C7H6NO2S)4(H2O)2]n, the two Ni atoms occupy inversion centers: one is covalently bonded to two monodentate carboxylate anions, and coordinated by two water molecules and by the pyridyl N atoms of another two carboxylate anions; the second Ni atom is chelated by two carboxylate anions and is also coordinated by the pyridyl N atoms of two carboxylate anions. Both Ni atoms are six-coordinate in distorted octahedral geometries.
Supporting information
CCDC reference: 245120
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (C-C) = 0.005 Å
- R factor = 0.048
- wR factor = 0.123
- Data-to-parameter ratio = 15.1
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 ............ 2.00 Ratio
PLAT127_ALERT_1_C Implicit Hall Symbol Inconsistent with Expl .... -P 2ya
PLAT128_ALERT_4_C Non-standard setting of Space group P21/c .... P21/a
PLAT152_ALERT_1_C Supplied and Calc Volume s.u. Inconsistent ..... ?
PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 2
PLAT731_ALERT_1_C Bond Calc 0.86(3), Rep 0.850(10) ...... 3.00 su-Rat
O1W -H1W1 1.555 1.555
PLAT731_ALERT_1_C Bond Calc 0.85(3), Rep 0.850(10) ...... 3.00 su-Rat
O1W -H1W2 1.555 1.555
PLAT735_ALERT_1_C D-H Calc 0.85(3), Rep 0.850(10) ...... 3.00 su-Rat
O1W -H2# 1.555 1.555
PLAT735_ALERT_1_C D-H Calc 0.86(3), Rep 0.850(10) ...... 3.00 su-Rat
O1W -H1# 1.555 1.555
0 ALERT level A = In general: serious problem
0 ALERT level B = Potentially serious problem
11 ALERT level C = Check and explain
0 ALERT level G = General alerts; check
9 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
0 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
2 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: ORTEPII (Johnson, 1976); software used to prepare material for publication: SHELXL97.
Poly[[diaquanickel(II)]-µ-(4-pyridysulfanyl)acetato-nickel(II)-tri-
µ-(4-pyridysulfanyl)acetato]
top
Crystal data top
[Ni2(C7H6NO2S)4(H2O)2] | F(000) = 848 |
Mr = 826.20 | Dx = 1.807 Mg m−3 |
Monoclinic, P21/a | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ya | Cell parameters from 3044 reflections |
a = 15.775 (1) Å | θ = 2.4–28.3° |
b = 5.7314 (4) Å | µ = 1.58 mm−1 |
c = 16.950 (1) Å | T = 293 K |
β = 97.726 (1)° | Plate, pale blue |
V = 1518.6 (2) Å3 | 0.19 × 0.13 × 0.03 mm |
Z = 2 | |
Data collection top
Bruker APEX area-detector diffractometer | 3436 independent reflections |
Radiation source: fine-focus sealed tube | 3052 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.029 |
φ and ω scans | θmax = 27.5°, θmin = 1.2° |
Absorption correction: multi-scan (SADABS; Bruker, 2002) | h = −20→19 |
Tmin = 0.791, Tmax = 0.954 | k = −7→5 |
8645 measured reflections | l = −21→22 |
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)] = 0.048 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.123 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.13 | w = 1/[σ2(Fo2) + (0.0641P)2 + 0.8297P] where P = (Fo2 + 2Fc2)/3 |
3436 reflections | (Δ/σ)max = 0.001 |
228 parameters | Δρmax = 0.69 e Å−3 |
3 restraints | Δρmin = −0.44 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 | 0.0135 (2) | |
Ni2 | 0.5000 | 0.5000 | 1.0000 | 0.0133 (2) | |
S1 | 0.26539 (5) | 0.2913 (2) | 0.65254 (5) | 0.0222 (2) | |
S2 | 0.62588 (5) | 1.0821 (1) | 0.82686 (4) | 0.0179 (2) | |
O1 | 0.4136 (1) | 0.3410 (4) | 0.5661 (1) | 0.0187 (5) | |
O2 | 0.3775 (1) | 0.6599 (4) | 0.4993 (1) | 0.0162 (5) | |
O3 | 0.5790 (1) | 0.7346 (4) | 0.9497 (1) | 0.0164 (5) | |
O4 | 0.6920 (2) | 0.5073 (4) | 0.9399 (1) | 0.0224 (5) | |
O1w | 0.4158 (2) | 0.7740 (4) | 0.9994 (1) | 0.0175 (5) | |
N1 | 0.4356 (2) | 0.4287 (5) | 0.8855 (1) | 0.0144 (5) | |
N2 | 0.5423 (2) | 0.6867 (4) | 0.5996 (2) | 0.0155 (5) | |
C1 | 0.3620 (2) | 0.5023 (5) | 0.5469 (2) | 0.0157 (6) | |
C2 | 0.2792 (2) | 0.5177 (6) | 0.5830 (2) | 0.0194 (7) | |
C3 | 0.3355 (2) | 0.3564 (5) | 0.7382 (2) | 0.0160 (6) | |
C4 | 0.3838 (2) | 0.5570 (6) | 0.7535 (2) | 0.0177 (6) | |
C5 | 0.4321 (2) | 0.5854 (6) | 0.8266 (2) | 0.0177 (6) | |
C6 | 0.3901 (2) | 0.2322 (5) | 0.8698 (2) | 0.0195 (7) | |
C7 | 0.3401 (2) | 0.1916 (6) | 0.7986 (2) | 0.0208 (7) | |
C8 | 0.6512 (2) | 0.6922 (5) | 0.9292 (2) | 0.0150 (6) | |
C9 | 0.6951 (2) | 0.8906 (6) | 0.8899 (2) | 0.0175 (6) | |
C10 | 0.5936 (2) | 0.9147 (5) | 0.7429 (2) | 0.0147 (6) | |
C11 | 0.5346 (2) | 1.0146 (5) | 0.6843 (2) | 0.0182 (7) | |
C12 | 0.5112 (2) | 0.8971 (5) | 0.6144 (2) | 0.0169 (6) | |
C13 | 0.5964 (2) | 0.5885 (6) | 0.6573 (2) | 0.0164 (6) | |
C14 | 0.6230 (2) | 0.6933 (6) | 0.7288 (2) | 0.0176 (6) | |
H1w1 | 0.374 (2) | 0.707 (6) | 1.018 (2) | 0.05 (1)* | |
H1w2 | 0.429 (2) | 0.899 (4) | 1.025 (2) | 0.05 (1)* | |
H2a | 0.2316 | 0.5130 | 0.5404 | 0.023* | |
H2b | 0.2774 | 0.6671 | 0.6097 | 0.023* | |
H4 | 0.3836 | 0.6715 | 0.7146 | 0.021* | |
H5 | 0.4642 | 0.7213 | 0.8356 | 0.021* | |
H6 | 0.3926 | 0.1183 | 0.9091 | 0.023* | |
H7 | 0.3093 | 0.0534 | 0.7907 | 0.025* | |
H9a | 0.7359 | 0.8227 | 0.8585 | 0.021* | |
H9b | 0.7272 | 0.9834 | 0.9316 | 0.021* | |
H11 | 0.5111 | 1.1601 | 0.6924 | 0.022* | |
H12 | 0.4720 | 0.9666 | 0.5755 | 0.020* | |
H13 | 0.6172 | 0.4403 | 0.6485 | 0.020* | |
H14 | 0.6604 | 0.6168 | 0.7674 | 0.021* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Ni1 | 0.0144 (3) | 0.0143 (3) | 0.0116 (3) | 0.0022 (2) | 0.0011 (2) | −0.0008 (2) |
Ni2 | 0.0163 (3) | 0.0125 (3) | 0.0110 (3) | 0.0008 (2) | 0.0022 (2) | 0.0002 (2) |
S1 | 0.0197 (4) | 0.0319 (5) | 0.0144 (4) | −0.0109 (3) | 0.0009 (3) | −0.0005 (3) |
S2 | 0.0257 (4) | 0.0157 (4) | 0.0122 (3) | −0.0017 (3) | 0.0018 (3) | −0.0020 (3) |
O1 | 0.018 (1) | 0.018 (1) | 0.021 (1) | 0.003 (1) | 0.004 (1) | 0.001 (1) |
O2 | 0.018 (1) | 0.019 (1) | 0.012 (1) | 0.002 (1) | 0.001 (1) | 0.003 (1) |
O3 | 0.018 (1) | 0.016 (1) | 0.016 (1) | −0.002 (1) | 0.005 (1) | 0.002 (1) |
O4 | 0.022 (1) | 0.021 (1) | 0.025 (1) | 0.003 (1) | 0.003 (1) | −0.001 (1) |
O1w | 0.020 (1) | 0.016 (1) | 0.017 (1) | 0.003 (1) | 0.004 (1) | −0.001 (1) |
N1 | 0.017 (1) | 0.013 (1) | 0.013 (1) | 0.002 (1) | 0.001 (1) | 0.001 (1) |
N2 | 0.015 (1) | 0.016 (1) | 0.015 (1) | 0.000 (1) | 0.000 (1) | −0.002 (1) |
C1 | 0.016 (2) | 0.020 (2) | 0.011 (1) | 0.000 (1) | −0.003 (1) | −0.004 (1) |
C2 | 0.015 (2) | 0.029 (2) | 0.014 (2) | 0.002 (1) | 0.000 (1) | 0.000 (1) |
C3 | 0.015 (2) | 0.019 (2) | 0.015 (1) | −0.00 (1) | 0.003 (1) | −0.001 (1) |
C4 | 0.022 (2) | 0.018 (2) | 0.014 (1) | −0.003 (1) | 0.005 (1) | 0.002 (1) |
C5 | 0.019 (2) | 0.017 (2) | 0.017 (2) | −0.003 (1) | 0.004 (1) | −0.001 (1) |
C6 | 0.027 (2) | 0.015 (2) | 0.016 (1) | −0.001 (1) | 0.002 (1) | 0.001 (1) |
C7 | 0.025 (2) | 0.017 (2) | 0.021 (2) | −0.006 (1) | 0.002 (1) | −0.003 (1) |
C8 | 0.017 (2) | 0.018 (2) | 0.009 (1) | −0.002 (1) | −0.002 (1) | −0.005 (1) |
C9 | 0.020 (2) | 0.022 (2) | 0.011 (1) | −0.003 (1) | 0.002 (1) | −0.003 (1) |
C10 | 0.017 (2) | 0.016 (2) | 0.012 (1) | −0.003 (1) | 0.006 (1) | −0.002 (1) |
C11 | 0.024 (2) | 0.011 (2) | 0.020 (2) | 0.002 (1) | 0.004 (1) | 0.000 (1) |
C12 | 0.018 (2) | 0.016 (2) | 0.016 (1) | 0.001 (1) | −0.001 (1) | 0.002 (1) |
C13 | 0.016 (2) | 0.017 (2) | 0.017 (1) | 0.004 (1) | 0.003 (1) | −0.002 (1) |
C14 | 0.019 (2) | 0.018 (2) | 0.016 (1) | 0.002 (1) | 0.001 (1) | −0.001 (1) |
Geometric parameters (Å, º) top
Ni1—N2 | 2.035 (2) | C1—C2 | 1.518 (4) |
Ni1—N2i | 2.035 (2) | C3—C4 | 1.385 (4) |
Ni1—O1 | 2.086 (2) | C3—C7 | 1.388 (4) |
Ni1—O1i | 2.086 (2) | C4—C5 | 1.374 (4) |
Ni1—O2 | 2.138 (2) | C6—C7 | 1.369 (4) |
Ni1—O2i | 2.138 (2) | C8—C9 | 1.529 (4) |
Ni2—N1 | 2.106 (2) | C10—C14 | 1.383 (4) |
Ni2—N1ii | 2.106 (2) | C10—C11 | 1.390 (4) |
Ni2—O3 | 2.091 (2) | C11—C12 | 1.369 (4) |
Ni2—O3ii | 2.091 (2) | C13—C14 | 1.366 (4) |
Ni2—O1w | 2.057 (2) | O1w—H1w1 | 0.85 (1) |
Ni2—O1wii | 2.057 (2) | O1w—H1w2 | 0.85 (1) |
S1—C3 | 1.743 (3) | C2—H2a | 0.97 |
S1—C2 | 1.786 (3) | C2—H2b | 0.97 |
S2—C10 | 1.736 (3) | C4—H4 | 0.93 |
S2—C9 | 1.797 (3) | C5—H5 | 0.93 |
O1—C1 | 1.246 (4) | C6—H6 | 0.93 |
O2—C1 | 1.256 (4) | C7—H7 | 0.93 |
O3—C8 | 1.259 (4) | C9—H9a | 0.97 |
O4—C8 | 1.241 (4) | C9—H9b | 0.97 |
N1—C5 | 1.340 (4) | C11—H11 | 0.93 |
N1—C6 | 1.343 (4) | C12—H12 | 0.93 |
N2—C13 | 1.333 (4) | C13—H13 | 0.93 |
N2—C12 | 1.338 (4) | C14—H14 | 0.93 |
| | | |
N2—Ni1—N2i | 180 | C4—C3—S1 | 127.2 (2) |
N2—Ni1—O1 | 87.08 (9) | C7—C3—S1 | 115.7 (2) |
N2—Ni1—O1i | 92.92 (9) | C5—C4—C3 | 119.4 (3) |
N2—Ni1—O2 | 88.52 (9) | N1—C5—C4 | 123.7 (3) |
N2—Ni1—O2i | 91.48 (9) | N1—C6—C7 | 123.1 (3) |
N2i—Ni1—O1 | 92.92 (9) | C6—C7—C3 | 120.1 (3) |
N2i—Ni1—O1i | 87.08 (9) | O4—C8—O3 | 126.5 (3) |
N2i—Ni1—O2 | 91.48 (9) | O4—C8—C9 | 116.3 (3) |
N2i—Ni1—O2i | 88.52 (9) | O3—C8—C9 | 117.2 (3) |
O1—Ni1—O1i | 180 | C8—C9—S2 | 116.0 (2) |
O1—Ni1—O2 | 62.27 (8) | C14—C10—C11 | 117.6 (3) |
O1—Ni1—O2i | 117.73 (8) | C14—C10—S2 | 125.5 (2) |
O1i—Ni1—O2 | 117.73 (8) | C11—C10—S2 | 117.0 (2) |
O1i—Ni1—O2i | 62.27 (8) | C12—C11—C10 | 119.5 (3) |
O2—Ni1—O2i | 180 | N2—C12—C11 | 122.8 (3) |
N1—Ni2—N1ii | 180 | N2—C13—C14 | 123.7 (3) |
N1—Ni2—O3 | 89.37 (9) | C13—C14—C10 | 119.1 (3) |
N1—Ni2—O3ii | 90.63 (9) | Ni2—O1w—H1w1 | 100 (3) |
N1—Ni2—O1w | 85.00 (9) | Ni2—O1w—H1w2 | 122 (3) |
N1—Ni2—O1wii | 95.00 (9) | H1w1—O1w—H1w2 | 109 (2) |
N1ii—Ni2—O3 | 90.63 (9) | C1—C2—H2a | 108.7 |
N1ii—Ni2—O3ii | 89.37 (9) | S1—C2—H2a | 108.7 |
N1ii—Ni2—O1w | 95.00 (9) | C1—C2—H2b | 108.7 |
N1ii—Ni2—O1wii | 85.00 (9) | S1—C2—H2b | 108.7 |
O3—Ni2—O3ii | 180 | H2a—C2—H2b | 107.6 |
O3—Ni2—O1w | 85.81 (9) | C5—C4—H4 | 120.3 |
O3—Ni2—O1wii | 94.19 (9) | C3—C4—H4 | 120.3 |
O3ii—Ni2—O1w | 94.19 (9) | N1—C5—H5 | 118.1 |
O3ii—Ni2—O1wii | 85.81 (9) | C4—C5—H5 | 118.1 |
O1w—Ni2—O1wii | 180 | N1—C6—H6 | 118.4 |
C3—S1—C2 | 105.9 (2) | C7—C6—H6 | 118.4 |
C10—S2—C9 | 103.8 (2) | C6—C7—H7 | 119.9 |
C1—O1—Ni1 | 89.2 (2) | C3—C7—H7 | 119.9 |
C1—O2—Ni1 | 86.7 (2) | C8—C9—H9a | 108.3 |
C8—O3—Ni2 | 126.8 (2) | S2—C9—H9a | 108.3 |
C5—N1—C6 | 116.5 (3) | C8—C9—H9b | 108.3 |
C5—N1—Ni2 | 121.6 (2) | S2—C9—H9b | 108.3 |
C6—N1—Ni2 | 121.6 (2) | H9a—C9—H9b | 107.4 |
C13—N2—C12 | 117.3 (3) | C12—C11—H11 | 120.3 |
C13—N2—Ni1 | 119.5 (2) | C10—C11—H11 | 120.3 |
C12—N2—Ni1 | 122.8 (2) | N2—C12—H12 | 118.6 |
O1—C1—O2 | 121.7 (3) | C11—C12—H12 | 118.6 |
O1—C1—C2 | 120.4 (3) | N2—C13—H13 | 118.2 |
O2—C1—C2 | 118.0 (3) | C14—C13—H13 | 118.2 |
C1—C2—S1 | 114.3 (2) | C13—C14—H14 | 120.5 |
C4—C3—C7 | 117.0 (3) | C10—C14—H14 | 120.5 |
| | | |
N2—Ni1—O1—C1 | 87.4 (2) | O1—C1—C2—S1 | 0.2 (4) |
N2i—Ni1—O1—C1 | −92.6 (2) | O2—C1—C2—S1 | −177.8 (2) |
O2—Ni1—O1—C1 | −2.4 (2) | C3—S1—C2—C1 | 73.5 (3) |
O2i—Ni1—O1—C1 | 177.6 (1) | C2—S1—C3—C4 | 7.5 (3) |
N2—Ni1—O2—C1 | −85.1 (2) | C2—S1—C3—C7 | −175.2 (3) |
N2i—Ni1—O2—C1 | 94.9 (2) | C7—C3—C4—C5 | −1.1 (5) |
O1—Ni1—O2—C1 | 2.4 (2) | S1—C3—C4—C5 | 176.1 (3) |
O1i—Ni1—O2—C1 | −177.6 (2) | C6—N1—C5—C4 | 1.5 (5) |
O1wii—Ni2—O3—C8 | 0.9 (2) | Ni2—N1—C5—C4 | −173.1 (2) |
O1w—Ni2—O3—C8 | −179.1 (2) | C3—C4—C5—N1 | −0.1 (5) |
N1—Ni2—O3—C8 | −94.1 (2) | C5—N1—C6—C7 | −1.8 (5) |
N1ii—Ni2—O3—C8 | 85.9 (2) | Ni2—N1—C6—C7 | 172.8 (3) |
O1w—Ni2—N1—C5 | 59.4 (2) | N1—C6—C7—C3 | 0.7 (5) |
O3ii—Ni2—N1—C5 | 153.6 (2) | C4—C3—C7—C6 | 0.8 (5) |
O3—Ni2—N1—C5 | −26.4 (2) | S1—C3—C7—C6 | −176.7 (3) |
O1wii—Ni2—N1—C6 | 65.1 (2) | Ni2—O3—C8—O4 | −5.4 (4) |
O1w—Ni2—N1—C6 | −114.9 (2) | Ni2—O3—C8—C9 | 177.2 (2) |
O3ii—Ni2—N1—C6 | −20.7 (2) | O4—C8—C9—S2 | 147.2 (2) |
O3—Ni2—N1—C6 | 159.3 (2) | O3—C8—C9—S2 | −35.1 (3) |
O1—Ni1—N2—C13 | 79.8 (2) | C10—S2—C9—C8 | −72.7 (2) |
O2—Ni1—N2—C13 | 142.1 (2) | C9—S2—C10—C14 | −5.1 (3) |
O2i—Ni1—N2—C13 | −37.9 (2) | C9—S2—C10—C11 | 176.5 (2) |
C1i—Ni1—N2—C13 | −69.1 (2) | C14—C10—C11—C12 | −3.0 (5) |
O1—Ni1—N2—C12 | −92.6 (3) | S2—C10—C11—C12 | 175.5 (2) |
O1i—Ni1—N2—C12 | 87.4 (3) | C13—N2—C12—C11 | 1.9 (5) |
O2—Ni1—N2—C12 | −30.3 (2) | Ni1—N2—C12—C11 | 174.5 (2) |
O2i—Ni1—N2—C12 | 149.7 (2) | C10—C11—C12—N2 | 0.5 (5) |
C1i—Ni1—N2—C12 | 118.5 (3) | C12—N2—C13—C14 | −1.8 (5) |
Ni1—O1—C1—O2 | 4.3 (3) | Ni1—N2—C13—C14 | −174.7 (2) |
Ni1—O1—C1—C2 | −173.7 (3) | N2—C13—C14—C10 | −0.7 (5) |
Ni1—O2—C1—O1 | −4.2 (3) | C11—C10—C14—C13 | 3.1 (5) |
Ni1—O2—C1—C2 | 173.8 (2) | S2—C10—C14—C13 | −175.3 (2) |
Symmetry codes: (i) −x+1, −y+1, −z+1; (ii) −x+1, −y+1, −z+2. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O1w—H1w2···O3iii | 0.85 (1) | 2.15 (2) | 2.943 (3) | 155 (4) |
O1w—H1w1···O4ii | 0.85 (1) | 1.82 (2) | 2.648 (3) | 163 (4) |
Symmetry codes: (ii) −x+1, −y+1, −z+2; (iii) −x+1, −y+2, −z+2. |