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The Mn atom and the coordinated water molecule in the title compound, [Mn(C7H6NO2S)2(H2O)]n, lie on a twofold axis; the Mn atom is chelated by the carboxyl –CO2 units and is also coordinated by the pyridyl N atoms of two adjacent anionic groups in a seven-coordinate trans-pentagonal bipyramidal geometry. The polymeric chain runs in a zigzag manner along the c axis, and neighboring chains are linked into a hydrogen-bonded layer structure.
Supporting information
CCDC reference: 234797
Key indicators
- Single-crystal X-ray study
- T = 298 K
- Mean (C-C) = 0.007 Å
- R factor = 0.054
- wR factor = 0.131
- Data-to-parameter ratio = 15.2
checkCIF/PLATON results
No syntax errors found
Alert level B
ABSTM02_ALERT_3_B The ratio of expected to reported Tmax/Tmin(RR') is < 0.75
Tmin and Tmax reported: 0.525 0.936
Tmin' and Tmax expected: 0.903 0.936
RR' = 0.581
Please check that your absorption correction is appropriate.
PLAT061_ALERT_3_B Tmax/Tmin Range Test RR' too Large ............. 0.58
Alert level C
PLAT029_ALERT_3_C _diffrn_measured_fraction_theta_full Low ....... 0.96
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ?
PLAT152_ALERT_1_C Supplied and Calc Volume s.u. Inconsistent ..... ?
PLAT341_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 7
PLAT731_ALERT_1_C Bond Calc 1.378(11), Rep 1.378(5) ...... 2.20 su-Rat
C4 -C5 1.555 1.555
Alert level G
FORMU01_ALERT_1_G There is a discrepancy between the atom counts in the
_chemical_formula_sum and _chemical_formula_moiety. This is
usually due to the moiety formula being in the wrong format.
Atom count from _chemical_formula_sum: C14 H14 Mn1 N2 O5 S2
Atom count from _chemical_formula_moiety:C140 H120 Mn20 N20 O40 S20
0 ALERT level A = In general: serious problem
2 ALERT level B = Potentially serious problem
5 ALERT level C = Check and explain
1 ALERT level G = General alerts; check
4 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
4 ALERT type 3 Indicator that the structure quality may be low
0 ALERT type 4 Improvement, methodology, query or suggestion
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[[aquamanganese(II)]-di-µ-4-pyridylthioacetato-
κ6O,
O':
N;N:
O,
O']
top
Crystal data top
[Mn(C7H6NO2S)2(H2O)] | F(000) = 836 |
Mr = 409.33 | Dx = 1.693 Mg m−3 |
Monoclinic, C2/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -C 2yc | Cell parameters from 950 reflections |
a = 21.595 (3) Å | θ = 2.5–24.7° |
b = 6.4904 (8) Å | µ = 1.11 mm−1 |
c = 15.611 (2) Å | T = 298 K |
β = 132.774 (1)° | Block, colorless |
V = 1606.1 (3) Å3 | 0.09 × 0.08 × 0.06 mm |
Z = 4 | |
Data collection top
Bruker APEX area-detector diffractometer | 1692 independent reflections |
Radiation source: fine-focus sealed tube | 1419 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.034 |
φ and ω scans | θmax = 27.0°, θmin = 2.6° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −27→27 |
Tmin = 0.525, Tmax = 0.936 | k = −8→5 |
4507 measured reflections | l = −19→19 |
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)] = 0.054 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.131 | H-atom parameters constrained |
S = 1.12 | w = 1/[σ2(Fo2) + (0.0629P)2 + 0.9714P] where P = (Fo2 + 2Fc2)/3 |
1692 reflections | (Δ/σ)max < 0.001 |
111 parameters | Δρmax = 0.60 e Å−3 |
0 restraints | Δρmin = −0.38 e Å−3 |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Mn1 | 0.0000 | 0.2092 (1) | 0.2500 | 0.0226 (2) | |
S1 | 0.22100 (6) | 0.7311 (1) | 0.58383 (9) | 0.0323 (3) | |
O1 | 0.0817 (2) | 0.5009 (4) | 0.3670 (2) | 0.0370 (6) | |
O2 | 0.1290 (1) | 0.1888 (4) | 0.4352 (2) | 0.0328 (6) | |
O1w | 0.0000 | −0.1325 (6) | 0.2500 | 0.0356 (8) | |
N1 | 0.0628 (2) | 0.7750 (4) | 0.6781 (3) | 0.0279 (7) | |
C1 | 0.1381 (2) | 0.3822 (6) | 0.4455 (3) | 0.0240 (7) | |
C2 | 0.2215 (2) | 0.4632 (5) | 0.5558 (3) | 0.0265 (7) | |
C3 | 0.1568 (2) | 0.7361 (5) | 0.6149 (3) | 0.0254 (7) | |
C4 | 0.1324 (3) | 0.5656 (6) | 0.6388 (4) | 0.0387 (9) | |
C5 | 0.0866 (3) | 0.5917 (6) | 0.6700 (4) | 0.041 (1) | |
C6 | 0.0847 (2) | 0.9386 (6) | 0.6518 (3) | 0.0327 (8) | |
C7 | 0.1307 (2) | 0.9269 (5) | 0.6208 (3) | 0.0328 (8) | |
H1w | −0.0423 | −0.1746 | 0.1856 | 0.043* | |
H2a | 0.2637 | 0.4416 | 0.5513 | 0.032* | |
H2b | 0.2383 | 0.3835 | 0.6213 | 0.032* | |
H4 | 0.1469 | 0.4341 | 0.6340 | 0.046* | |
H5 | 0.0713 | 0.4747 | 0.6864 | 0.050* | |
H6 | 0.0677 | 1.0681 | 0.6547 | 0.039* | |
H7 | 0.1444 | 1.0463 | 0.6037 | 0.039* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Mn1 | 0.0269 (4) | 0.0211 (4) | 0.0277 (4) | 0.000 | 0.0217 (3) | 0.000 |
S1 | 0.0416 (5) | 0.0279 (5) | 0.0486 (6) | −0.0067 (4) | 0.0390 (5) | −0.0071 (4) |
O1 | 0.031 (1) | 0.035 (2) | 0.032 (1) | 0.008 (1) | 0.016 (1) | 0.007 (1) |
O2 | 0.035 (1) | 0.026 (2) | 0.041 (1) | 0.002 (1) | 0.027 (1) | 0.001 (1) |
O1w | 0.037 (2) | 0.023 (2) | 0.032 (2) | 0.000 | 0.018 (2) | 0.000 |
N1 | 0.034 (2) | 0.031 (2) | 0.032 (2) | 0.002 (1) | 0.027 (1) | −0.001 (1) |
C1 | 0.027 (2) | 0.032 (2) | 0.028 (2) | 0.004 (1) | 0.025 (2) | 0.001 (1) |
C2 | 0.026 (2) | 0.029 (2) | 0.030 (2) | 0.004 (1) | 0.021 (2) | 0.002 (1) |
C3 | 0.028 (2) | 0.030 (2) | 0.025 (2) | −0.003 (1) | 0.021 (2) | −0.003 (1) |
C4 | 0.061 (2) | 0.021 (2) | 0.066 (3) | 0.003 (2) | 0.056 (2) | −0.001 (2) |
C5 | 0.064 (3) | 0.027 (2) | 0.068 (3) | −0.006 (2) | 0.059 (3) | −0.003 (2) |
C6 | 0.043 (2) | 0.025 (2) | 0.040 (2) | 0.008 (2) | 0.032 (2) | 0.006 (2) |
C7 | 0.048 (2) | 0.023 (2) | 0.048 (2) | 0.002 (2) | 0.041 (2) | 0.005 (2) |
Geometric parameters (Å, º) top
Mn1—O1 | 2.378 (3) | C1—C2 | 1.508 (5) |
Mn1—O1i | 2.378 (3) | C3—C4 | 1.380 (5) |
Mn1—O2 | 2.280 (2) | C3—C7 | 1.389 (5) |
Mn1—O2i | 2.280 (2) | C4—C5 | 1.378 (5) |
Mn1—O1w | 2.218 (4) | C6—C7 | 1.371 (5) |
Mn1—N1ii | 2.276 (3) | O1w—H1w | 0.82 |
Mn1—N1iii | 2.276 (3) | C2—H2a | 0.97 |
S1—C3 | 1.754 (3) | C2—H2b | 0.97 |
S1—C2 | 1.795 (4) | C4—H4 | 0.93 |
O1—C1 | 1.246 (4) | C5—H5 | 0.93 |
O2—C1 | 1.264 (4) | C6—H6 | 0.93 |
N1—C6 | 1.335 (4) | C7—H7 | 0.93 |
N1—C5 | 1.335 (4) | | |
| | | |
O1—Mn1—O1i | 74.5 (1) | C5—N1—Mn1ii | 118.9 (2) |
O1—Mn1—O2 | 56.1 (1) | O1—C1—O2 | 121.7 (3) |
O1—Mn1—O2i | 130.6 (1) | O1—C1—C2 | 121.3 (3) |
O1—Mn1—O1w | 142.8 (1) | O2—C1—C2 | 116.9 (3) |
O1—Mn1—N1ii | 88.0 (1) | C1—C2—S1 | 114.5 (2) |
O1—Mn1—N1iii | 87.9 (1) | C4—C3—C7 | 116.9 (3) |
O1i—Mn1—O2 | 130.6 (1) | C4—C3—S1 | 125.3 (3) |
O1i—Mn1—O2i | 56.1 (1) | C7—C3—S1 | 117.8 (3) |
O1i—Mn1—O1w | 142.8 (1) | C5—C4—C3 | 119.6 (3) |
O1i—Mn1—N1ii | 87.9 (1) | N1—C5—C4 | 123.9 (3) |
O1i—Mn1—N1iii | 88.0 (1) | N1—C6—C7 | 123.9 (3) |
O2—Mn1—O2i | 173.3 (1) | C6—C7—C3 | 119.7 (3) |
O2—Mn1—O1w | 86.7 (1) | Mn1—O1w—H1w | 109.5 |
O2—Mn1—N1ii | 90.1 (1) | C1—C2—H2a | 108.6 |
O2—Mn1—N1iii | 90.2 (1) | S1—C2—H2a | 108.6 |
O2i—Mn1—O1w | 86.7 (1) | C1—C2—H2b | 108.6 |
O2i—Mn1—N1ii | 90.2 (1) | S1—C2—H2b | 108.6 |
O2i—Mn1—N1iii | 90.1 (1) | H2a—C2—H2b | 107.6 |
O1w—Mn1—N1ii | 92.6 (1) | C5—C4—H4 | 120.2 |
O1w—Mn1—N1iii | 92.6 (1) | C3—C4—H4 | 120.2 |
N1ii—Mn1—N1iii | 174.9 (2) | N1—C5—H5 | 118.1 |
C3—S1—C2 | 102.9 (2) | C4—C5—H5 | 118.1 |
C1—O1—Mn1 | 89.0 (2) | N1—C6—H6 | 118.1 |
C1—O2—Mn1 | 93.1 (2) | C7—C6—H6 | 118.1 |
C6—N1—C5 | 116.1 (3) | C6—C7—H7 | 120.2 |
C6—N1—Mn1ii | 124.7 (2) | C3—C7—H7 | 120.2 |
| | | |
O1w—Mn1—O1—C1 | 1.5 (2) | O1—C1—C2—S1 | 18.0 (4) |
N1iii—Mn1—O1—C1 | −90.0 (2) | O2—C1—C2—S1 | −163.9 (2) |
N1ii—Mn1—O1—C1 | 93.1 (2) | C3—S1—C2—C1 | 68.4 (3) |
O2—Mn1—O1—C1 | 1.7 (2) | C2—S1—C3—C4 | 13.9 (4) |
O2i—Mn1—O1—C1 | −178.3 (2) | C2—S1—C3—C7 | −168.9 (3) |
O1i—Mn1—O1—C1 | −178.5 (2) | C7—C3—C4—C5 | −1.8 (6) |
O1w—Mn1—O2—C1 | 178.3 (2) | S1—C3—C4—C5 | 175.4 (3) |
N1iii—Mn1—O2—C1 | 85.7 (2) | C6—N1—C5—C4 | 1.2 (6) |
N1ii—Mn1—O2—C1 | −89.2 (2) | Mn1ii—N1—C5—C4 | −173.4 (3) |
O1—Mn1—O2—C1 | −1.7 (2) | C3—C4—C5—N1 | 0.5 (7) |
O1i—Mn1—O2—C1 | −1.8 (2) | C5—N1—C6—C7 | −1.6 (6) |
Mn1—O1—C1—O2 | −2.9 (3) | Mn1ii—N1—C6—C7 | 172.6 (3) |
Mn1—O1—C1—C2 | 175.2 (2) | N1—C6—C7—C3 | 0.3 (6) |
Mn1—O2—C1—O1 | 3.1 (3) | C4—C3—C7—C6 | 1.4 (6) |
Mn1—O2—C1—C2 | −175.1 (2) | S1—C3—C7—C6 | −176.1 (3) |
Symmetry codes: (i) −x, y, −z+1/2; (ii) −x, −y+1, −z+1; (iii) x, −y+1, z−1/2. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O1w—H1w···O1iv | 0.82 | 2.21 | 2.781 (4) | 127 |
Symmetry code: (iv) −x, y−1, −z+1/2. |
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