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metal-organic compounds
The water-coordinated Ni atom in the title compound, [Ni(C7H6NO2S)2(H2O)]n, is covalently bonded to two carboxylate groups (one binding in a monodentate mode and the other in a chelating mode); it is also linked to the N atoms of two other carboxylate anions in an octahedral environment. The compound adopts a linear chain architecture; adjacent chains are linked into layers by hydrogen bonds.
Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536804013340/bt6463sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536804013340/bt6463Isup2.hkl |
CCDC reference: 245119
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (C-C) = 0.003 Å
- R factor = 0.035
- wR factor = 0.095
- Data-to-parameter ratio = 15.6
checkCIF/PLATON results
No syntax errors found
Alert level C ABSTM02_ALERT_3_C The ratio of expected to reported Tmax/Tmin(RR') is < 0.90 Tmin and Tmax reported: 0.665 0.864 Tmin' and Tmax expected: 0.818 0.860 RR' = 0.809 Please check that your absorption correction is appropriate. PLAT029_ALERT_3_C _diffrn_measured_fraction_theta_full Low ....... 0.96 PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT061_ALERT_3_C Tmax/Tmin Range Test RR' too Large ............. 0.81 PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 2 PLAT731_ALERT_1_C Bond Calc 0.85(3), Rep 0.850(10) ...... 3.00 su-Rat O1W -H1W1 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 0.84(3), Rep 0.840(10) ...... 3.00 su-Rat O1W -H1W2 1.555 1.555 PLAT735_ALERT_1_C D-H Calc 0.84(3), Rep 0.840(10) ...... 3.00 su-Rat O1W -H2# 1.555 1.555 PLAT735_ALERT_1_C D-H Calc 0.85(3), Rep 0.850(10) ...... 3.00 su-Rat O1W -H1# 1.555 1.555 PLAT736_ALERT_1_C H...A Calc 1.88(3), Rep 1.880(10) ...... 3.00 su-Rat H2# -O1 1.555 2.667
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 10 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 6 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 3 ALERT type 3 Indicator that the structure quality may be low 1 ALERT type 4 Improvement, methodology, query or suggestion
Computing details top
Data collection: SMART (Bruker, 2001); cell refinement: SAINT (Bruker, 2001); 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.
catena-Poly[[aquanickel(II)]-di-µ-(4-pyridylsulfanyl)acetato] top
Crystal data top
[Ni(C7H6NO2S)2(H2O)] | Z = 2 |
Mr = 413.10 | F(000) = 424 |
Triclinic, P1 | Dx = 1.723 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71073 Å |
a = 8.1693 (4) Å | Cell parameters from 5217 reflections |
b = 10.3430 (5) Å | θ = 2.8–26.3° |
c = 10.6876 (5) Å | µ = 1.51 mm−1 |
α = 67.371 (1)° | T = 293 K |
β = 73.176 (1)° | Prism, green |
γ = 86.825 (1)° | 0.13 × 0.12 × 0.10 mm |
V = 796.25 (7) Å3 |
Data collection top
Bruker APEX area-detector diffractometer | 3511 independent reflections |
Radiation source: fine-focus sealed tube | 3266 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.017 |
φ and ω scans | θmax = 27.5°, θmin = 2.1° |
Absorption correction: multi-scan (SADABS; Bruker, 2001) | h = −10→10 |
Tmin = 0.665, Tmax = 0.864 | k = −13→13 |
6789 measured reflections | l = −13→13 |
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)] = 0.035 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.095 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.06 | w = 1/[σ2(Fo2) + (0.056P)2 + 0.2563P] where P = (Fo2 + 2Fc2)/3 |
3511 reflections | (Δ/σ)max = 0.001 |
225 parameters | Δρmax = 0.49 e Å−3 |
2 restraints | Δρmin = −0.26 e Å−3 |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
x | y | z | Uiso*/Ueq | ||
Ni1 | 0.50718 (3) | 0.71247 (3) | 0.78110 (3) | 0.0259 (1) | |
S1 | 0.87796 (9) | 0.76461 (7) | 1.06171 (8) | 0.0427 (2) | |
S2 | 0.07987 (7) | 0.77873 (6) | 0.41886 (6) | 0.0340 (1) | |
O1 | 0.6400 (2) | 0.6852 (2) | 0.9294 (2) | 0.0308 (3) | |
O2 | 0.7493 (2) | 0.8390 (2) | 0.7145 (2) | 0.0379 (4) | |
O3 | 0.4218 (2) | 0.7779 (2) | 0.6082 (2) | 0.0318 (3) | |
O4 | 0.1770 (2) | 0.6469 (2) | 0.6941 (2) | 0.0396 (4) | |
O1w | 0.2967 (2) | 0.5799 (2) | 0.9134 (2) | 0.0336 (3) | |
N1 | 0.6162 (2) | 1.1238 (2) | 1.1669 (2) | 0.0301 (4) | |
N2 | 0.3642 (2) | 0.4463 (2) | 0.2762 (2) | 0.0304 (4) | |
C1 | 0.7555 (3) | 0.7773 (2) | 0.8382 (2) | 0.0294 (4) | |
C2 | 0.9081 (3) | 0.8081 (3) | 0.8771 (3) | 0.0384 (5) | |
C3 | 0.7725 (3) | 0.9048 (2) | 1.0942 (2) | 0.0310 (4) | |
C4 | 0.7327 (3) | 1.0240 (2) | 0.9941 (2) | 0.0371 (5) | |
C5 | 0.6569 (3) | 1.1294 (2) | 1.0348 (2) | 0.0376 (5) | |
C6 | 0.6526 (3) | 1.0068 (2) | 1.2639 (2) | 0.0326 (5) | |
C7 | 0.7296 (3) | 0.8973 (2) | 1.2329 (2) | 0.0349 (5) | |
C8 | 0.2769 (3) | 0.7468 (2) | 0.6042 (2) | 0.0275 (4) | |
C9 | 0.2249 (3) | 0.8486 (2) | 0.4777 (2) | 0.0345 (5) | |
C10 | 0.1975 (3) | 0.6541 (2) | 0.3642 (2) | 0.0282 (4) | |
C11 | 0.1141 (3) | 0.5710 (2) | 0.3235 (2) | 0.0329 (5) | |
C12 | 0.2002 (3) | 0.4707 (2) | 0.2810 (2) | 0.0328 (5) | |
C13 | 0.4442 (3) | 0.5272 (2) | 0.3149 (3) | 0.0358 (5) | |
C14 | 0.3678 (3) | 0.6307 (2) | 0.3585 (2) | 0.0340 (5) | |
H1w1 | 0.240 (3) | 0.583 (3) | 0.857 (3) | 0.06 (1)* | |
H1w2 | 0.320 (4) | 0.498 (2) | 0.959 (3) | 0.07 (1)* | |
H2a | 0.9418 | 0.9074 | 0.8268 | 0.046* | |
H2b | 1.0026 | 0.7572 | 0.8436 | 0.046* | |
H4 | 0.7568 | 1.0328 | 0.9005 | 0.045* | |
H5 | 0.6326 | 1.2094 | 0.9658 | 0.045* | |
H6 | 0.6239 | 0.9996 | 1.3572 | 0.039* | |
H7 | 0.7530 | 0.8187 | 1.3039 | 0.042* | |
H9a | 0.3279 | 0.8868 | 0.3992 | 0.041* | |
H9b | 0.1728 | 0.9260 | 0.5013 | 0.041* | |
H11 | 0.0000 | 0.5832 | 0.3250 | 0.039* | |
H12 | 0.1414 | 0.4164 | 0.2539 | 0.039* | |
H13 | 0.5584 | 0.5127 | 0.3123 | 0.043* | |
H14 | 0.4297 | 0.6844 | 0.3840 | 0.041* |
Atomic displacement parameters (Å2) top
U11 | U22 | U33 | U12 | U13 | U23 | |
Ni1 | 0.0293 (2) | 0.0241 (2) | 0.0255 (2) | 0.0018 (1) | −0.0103 (1) | −0.0092 (1) |
S1 | 0.0500 (4) | 0.0401 (3) | 0.0602 (4) | 0.0187 (3) | −0.0349 (3) | −0.0312 (3) |
S2 | 0.0364 (3) | 0.0368 (3) | 0.0390 (3) | 0.0133 (2) | −0.0199 (2) | −0.0202 (2) |
O1 | 0.033 (1) | 0.028 (1) | 0.032 (1) | 0.000 (1) | −0.014 (1) | −0.009 (1) |
O2 | 0.046 (1) | 0.030 (1) | 0.034 (1) | 0.001 (1) | −0.011 (1) | −0.008 (1) |
O3 | 0.035 (1) | 0.034 (1) | 0.028 (1) | 0.001 (1) | −0.013 (1) | −0.011 (1) |
O4 | 0.037 (1) | 0.041 (1) | 0.037 (1) | −0.001 (1) | −0.016 (1) | −0.006 (1) |
O1w | 0.036 (1) | 0.029 (1) | 0.031 (1) | 0.002 (1) | −0.010 (1) | −0.008 (1) |
N1 | 0.031 (1) | 0.028 (1) | 0.032 (1) | 0.002 (1) | −0.011 (1) | −0.012 (1) |
N2 | 0.031 (1) | 0.031 (1) | 0.032 (1) | 0.003 (1) | −0.010 (1) | −0.015 (1) |
C1 | 0.035 (1) | 0.020 (1) | 0.037 (1) | 0.006 (1) | −0.012 (1) | −0.015 (1) |
C2 | 0.031 (1) | 0.041 (1) | 0.052 (1) | 0.004 (1) | −0.009 (1) | −0.030 (1) |
C3 | 0.029 (1) | 0.030 (1) | 0.042 (1) | 0.004 (1) | −0.016 (1) | −0.018 (1) |
C4 | 0.045 (1) | 0.037 (1) | 0.032 (1) | 0.008 (1) | −0.012 (1) | −0.015 (1) |
C5 | 0.046 (1) | 0.032 (1) | 0.031 (1) | 0.008 (1) | −0.012 (1) | −0.009 (1) |
C6 | 0.039 (1) | 0.031 (1) | 0.031 (1) | 0.001 (1) | −0.015 (1) | −0.012 (1) |
C7 | 0.044 (1) | 0.028 (1) | 0.039 (1) | 0.005 (1) | −0.022 (1) | −0.012 (1) |
C8 | 0.032 (1) | 0.027 (1) | 0.029 (1) | 0.008 (1) | −0.012 (1) | −0.014 (1) |
C9 | 0.045 (1) | 0.028 (1) | 0.037 (1) | 0.006 (1) | −0.021 (1) | −0.013 (1) |
C10 | 0.032 (1) | 0.029 (1) | 0.026 (1) | 0.004 (1) | −0.011 (1) | −0.011 (1) |
C11 | 0.031 (1) | 0.038 (1) | 0.036 (1) | 0.005 (1) | −0.014 (1) | −0.017 (1) |
C12 | 0.032 (1) | 0.036 (1) | 0.036 (1) | 0.001 (1) | −0.013 (1) | −0.018 (1) |
C13 | 0.027 (1) | 0.041 (1) | 0.045 (1) | 0.004 (1) | −0.012 (1) | −0.021 (1) |
C14 | 0.028 (1) | 0.038 (1) | 0.045 (1) | 0.002 (1) | −0.013 (1) | −0.024 (1) |
Geometric parameters (Å, º) top
Ni1—O3 | 2.023 (2) | C4—C5 | 1.376 (3) |
Ni1—O1 | 2.094 (2) | C6—C7 | 1.370 (3) |
Ni1—O2 | 2.210 (2) | C8—C9 | 1.518 (3) |
Ni1—O1w | 2.049 (2) | C10—C11 | 1.384 (3) |
Ni1—N1i | 2.099 (2) | C10—C14 | 1.387 (3) |
Ni1—N2ii | 2.094 (2) | C11—C12 | 1.368 (3) |
S1—C3 | 1.743 (2) | C13—C14 | 1.377 (3) |
S1—C2 | 1.790 (3) | O1w—H1w1 | 0.85 (1) |
S2—C10 | 1.745 (2) | O1w—H1w2 | 0.84 (1) |
S2—C9 | 1.788 (2) | C2—H2a | 0.97 |
O1—C1 | 1.265 (3) | C2—H2b | 0.97 |
O2—C1 | 1.243 (3) | C4—H4 | 0.93 |
O3—C8 | 1.260 (3) | C5—H5 | 0.93 |
O4—C8 | 1.238 (3) | C6—H6 | 0.93 |
N1—C5 | 1.332 (3) | C7—H7 | 0.93 |
N1—C6 | 1.342 (3) | C9—H9a | 0.97 |
N2—C13 | 1.335 (3) | C9—H9b | 0.97 |
N2—C12 | 1.339 (3) | C11—H11 | 0.93 |
C1—C2 | 1.508 (3) | C12—H12 | 0.93 |
C3—C4 | 1.383 (3) | C13—H13 | 0.93 |
C3—C7 | 1.394 (3) | C14—H14 | 0.93 |
O1—Ni1—O2 | 60.84 (6) | O3—C8—C9 | 114.0 (2) |
O1—Ni1—O3 | 166.10 (6) | C8—C9—S2 | 116.3 (2) |
O1—Ni1—O1w | 98.41 (6) | C11—C10—C14 | 117.1 (2) |
O1—Ni1—N1i | 88.55 (6) | C11—C10—S2 | 117.5 (2) |
O1—Ni1—N2ii | 91.65 (6) | C14—C10—S2 | 125.5 (2) |
O2—Ni1—O3 | 105.37 (6) | C12—C11—C10 | 119.7 (2) |
O2—Ni1—O1w | 158.89 (7) | N2—C12—C11 | 123.8 (2) |
O2—Ni1—N1i | 86.52 (6) | N2—C13—C14 | 123.8 (2) |
O2—Ni1—N2ii | 92.02 (7) | C13—C14—C10 | 119.3 (2) |
O3—Ni1—N1i | 88.82 (7) | Ni1—O1w—H1w1 | 103 (2) |
O3—Ni1—N2ii | 90.56 (7) | Ni1—O1w—H1w2 | 114 (2) |
O3—Ni1—O1w | 95.20 (7) | H1w1—O1w—H1w2 | 113 (3) |
O1w—Ni1—N1i | 89.29 (7) | C1—C2—H2a | 108.3 |
O1w—Ni1—N2ii | 92.43 (7) | S1—C2—H2a | 108.3 |
N1i—Ni1—N2ii | 178.21 (7) | C1—C2—H2b | 108.3 |
C3—S1—C2 | 104.3 (1) | S1—C2—H2b | 108.3 |
C10—S2—C9 | 103.1 (1) | H2a—C2—H2b | 107.4 |
C1—O1—Ni1 | 91.5 (1) | C5—C4—H4 | 120.4 |
C1—O2—Ni1 | 86.8 (1) | C3—C4—H4 | 120.4 |
C8—O3—Ni1 | 126.4 (1) | N1—C5—H5 | 118.0 |
C5—N1—C6 | 116.5 (2) | C4—C5—H5 | 118.0 |
C5—N1—Ni1i | 120.9 (2) | N1—C6—H6 | 118.2 |
C6—N1—Ni1i | 122.5 (2) | C7—C6—H6 | 118.2 |
C13—N2—C12 | 116.2 (2) | C6—C7—H7 | 120.3 |
C13—N2—Ni1ii | 120.0 (2) | C3—C7—H7 | 120.3 |
C12—N2—Ni1ii | 123.7 (2) | C8—C9—H9a | 108.2 |
O2—C1—O1 | 120.9 (2) | S2—C9—H9a | 108.2 |
O2—C1—C2 | 119.1 (2) | C8—C9—H9b | 108.2 |
O1—C1—C2 | 119.9 (2) | S2—C9—H9b | 108.2 |
C1—C2—S1 | 116.1 (2) | H9a—C9—H9b | 107.4 |
C4—C3—C7 | 117.3 (2) | C12—C11—H11 | 120.1 |
C4—C3—S1 | 125.9 (2) | C10—C11—H11 | 120.1 |
C7—C3—S1 | 116.7 (2) | N2—C12—H12 | 118.1 |
C5—C4—C3 | 119.1 (2) | C11—C12—H12 | 118.1 |
N1—C5—C4 | 124.0 (2) | N2—C13—H13 | 118.1 |
N1—C6—C7 | 123.5 (2) | C14—C13—H13 | 118.1 |
C6—C7—C3 | 119.4 (2) | C13—C14—H14 | 120.3 |
O4—C8—O3 | 126.1 (2) | C10—C14—H14 | 120.3 |
O4—C8—C9 | 119.9 (2) | ||
O3—Ni1—O1—C1 | −7.4 (3) | C6—N1—C5—C4 | −0.2 (4) |
O1w—Ni1—O1—C1 | −175.6 (1) | Ni1i—N1—C5—C4 | −177.8 (2) |
N2ii—Ni1—O1—C1 | 91.7 (1) | C3—C4—C5—N1 | −1.0 (4) |
N1i—Ni1—O1—C1 | −86.5 (1) | C5—N1—C6—C7 | 0.9 (3) |
O2—Ni1—O1—C1 | 0.3 (1) | Ni1i—N1—C6—C7 | 178.5 (2) |
O3—Ni1—O2—C1 | 177.8 (1) | N1—C6—C7—C3 | −0.5 (4) |
O1w—Ni1—O2—C1 | 11.0 (2) | C4—C3—C7—C6 | −0.6 (3) |
N2ii—Ni1—O2—C1 | −91.1 (1) | S1—C3—C7—C6 | 177.5 (2) |
O1—Ni1—O2—C1 | −0.3 (1) | Ni1—O3—C8—O4 | −18.4 (3) |
N1i—Ni1—O2—C1 | 90.0 (1) | Ni1—O3—C8—C9 | 159.1 (1) |
O1w—Ni1—O3—C8 | 5.2 (2) | O4—C8—C9—S2 | −29.3 (3) |
N2ii—Ni1—O3—C8 | 97.7 (2) | O3—C8—C9—S2 | 153.0 (2) |
O1—Ni1—O3—C8 | −163.1 (2) | C10—S2—C9—C8 | −63.7 (2) |
N1i—Ni1—O3—C8 | −84.0 (2) | C9—S2—C10—C11 | 174.4 (2) |
O2—Ni1—O3—C8 | −170.0 (2) | C9—S2—C10—C14 | −5.3 (2) |
Ni1—O2—C1—O1 | 0.5 (2) | C14—C10—C11—C12 | 0.4 (3) |
Ni1—O2—C1—C2 | 177.2 (2) | S2—C10—C11—C12 | −179.4 (2) |
Ni1—O1—C1—O2 | −0.6 (2) | C13—N2—C12—C11 | −0.5 (3) |
Ni1—O1—C1—C2 | −177.2 (2) | Ni1ii—N2—C12—C11 | 177.5 (2) |
O2—C1—C2—S1 | 159.7 (2) | C10—C11—C12—N2 | 0.2 (4) |
O1—C1—C2—S1 | −23.6 (3) | C12—N2—C13—C14 | 0.2 (3) |
C3—S1—C2—C1 | −80.6 (2) | Ni1ii—N2—C13—C14 | −177.8 (2) |
C2—S1—C3—C4 | −3.2 (2) | N2—C13—C14—C10 | 0.3 (4) |
C2—S1—C3—C7 | 179.0 (2) | C11—C10—C14—C13 | −0.6 (3) |
C7—C3—C4—C5 | 1.3 (4) | S2—C10—C14—C13 | 179.1 (2) |
S1—C3—C4—C5 | −176.6 (2) |
Symmetry codes: (i) −x+1, −y+2, −z+2; (ii) −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—H1w2···O1iii | 0.84 (1) | 1.88 (1) | 2.722 (2) | 176 (3) |
O1w—H1w1···O4 | 0.85 (1) | 1.83 (2) | 2.633 (2) | 158 (3) |
Symmetry code: (iii) −x+1, −y+1, −z+2. |
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