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The crystal structure of the title compound, [Na(C
2H
3N
4S)(H
2O)
3]
n, features polymeric chains made up of sodium coordination octahedra NaS(H
2O)
5, each of them sharing two μ-H
2O
μ-H
2O edges with two adjacent octahedra; the chains run along the
a axis of the crystal structure. All three unsubstituted N atoms of the tetrazole ring are involved in the complex hydrogen-bonding system; however, none of them participate in the coordination of the sodium ion.
Supporting information
CCDC reference: 647478
Key indicators
- Single-crystal X-ray study
- T = 296 K
- Mean (N-C) = 0.002 Å
- R factor = 0.027
- wR factor = 0.072
- Data-to-parameter ratio = 11.6
checkCIF/PLATON results
No syntax errors found
Alert level C
PLAT154_ALERT_1_C The su's on the Cell Angles are Equal (x 10000) 100 Deg.
PLAT180_ALERT_3_C Check Cell Rounding: # of Values Ending with 0 = 4
PLAT731_ALERT_1_C Bond Calc 0.81(3), Rep 0.814(10) ...... 3.00 su-Ra
O2 -H2B 1.555 1.555
PLAT735_ALERT_1_C D-H Calc 0.81(3), Rep 0.814(10) ...... 3.00 su-Ra
O2 -H2B 1.555 1.555
PLAT764_ALERT_4_C Overcomplete CIF Bond List Detected (Rep/Expd) . 1.31 Ratio
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
3 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
1 ALERT type 3 Indicator that the structure quality may be low
1 ALERT type 4 Improvement, methodology, query or suggestion
0 ALERT type 5 Informative message, check
Data collection: APEX2 (Bruker, 2006); cell refinement: APEX2; data reduction: SAINT (Bruker, 2005); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: XSHELL (Bruker–Nonius, 2004) and DIAMOND (Brandenburg & Brendt, 2001); software used to prepare material for publication: SHELXTL (Bruker, 2003).
catena-Poly[[aqua(1-methyl-1
H-1,2,3,4-tetrazole-5-thiolato-
κS)sodium]di- µ-aqua-
κ4O:
O]
top
Crystal data top
[Na(C2H3N4S)(H2O)3] | Z = 2 |
Mr = 192.18 | F(000) = 200 |
Triclinic, P1 | Dx = 1.532 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71073 Å |
a = 6.4420 (7) Å | Cell parameters from 1954 reflections |
b = 7.0072 (8) Å | θ = 3.0–27.4° |
c = 9.7713 (11) Å | µ = 0.41 mm−1 |
α = 105.519 (1)° | T = 296 K |
β = 97.098 (1)° | Block, light yellow |
γ = 96.589 (1)° | 0.42 × 0.39 × 0.30 mm |
V = 416.67 (8) Å3 | |
Data collection top
Bruker SMART CCD area-detector diffractometer | 1463 independent reflections |
Radiation source: fine-focus sealed tube | 1401 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.013 |
ω scans | θmax = 25.1°, θmin = 3.0° |
Absorption correction: multi-scan (SADABS; Bruker, 2004) | h = −7→7 |
Tmin = 0.848, Tmax = 0.889 | k = −8→8 |
2105 measured reflections | l = −11→9 |
Refinement top
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.027 | H atoms treated by a mixture of independent and constrained refinement |
wR(F2) = 0.072 | w = 1/[σ2(Fo2) + (0.0406P)2 + 0.153P] where P = (Fo2 + 2Fc2)/3 |
S = 1.00 | (Δ/σ)max = 0.001 |
1463 reflections | Δρmax = 0.21 e Å−3 |
126 parameters | Δρmin = −0.26 e Å−3 |
6 restraints | Extinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
Primary atom site location: structure-invariant direct methods | Extinction coefficient: 0.505 (19) |
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 | |
Na1 | 0.26447 (9) | 0.61496 (9) | 0.48045 (7) | 0.0405 (2) | |
S1 | 0.13426 (6) | 0.98586 (5) | 0.66590 (4) | 0.03731 (18) | |
C5 | 0.1932 (2) | 0.9636 (2) | 0.83625 (15) | 0.0290 (3) | |
C6 | 0.2459 (3) | 1.3301 (2) | 0.97741 (19) | 0.0472 (4) | |
H6A | 0.3448 | 1.3731 | 0.9218 | 0.071* | |
H6B | 0.2902 | 1.4018 | 1.0773 | 0.071* | |
H6C | 0.1079 | 1.3567 | 0.9456 | 0.071* | |
N1 | 0.2051 (2) | 0.79578 (19) | 0.87565 (14) | 0.0358 (3) | |
N2 | 0.2579 (2) | 0.8520 (2) | 1.02108 (14) | 0.0395 (3) | |
N3 | 0.2783 (2) | 1.0441 (2) | 1.07220 (13) | 0.0380 (3) | |
N4 | 0.23792 (18) | 1.11692 (18) | 0.95878 (13) | 0.0316 (3) | |
O1 | −0.0991 (2) | 0.55115 (17) | 0.35986 (12) | 0.0416 (3) | |
O2 | 0.3843 (2) | 0.7499 (3) | 0.30507 (18) | 0.0645 (4) | |
O3 | 0.3691 (2) | 0.28641 (19) | 0.38347 (13) | 0.0449 (3) | |
H1A | −0.119 (3) | 0.657 (2) | 0.343 (2) | 0.060 (6)* | |
H1B | −0.133 (3) | 0.458 (2) | 0.2855 (15) | 0.056 (6)* | |
H2A | 0.496 (3) | 0.828 (3) | 0.326 (3) | 0.089 (9)* | |
H2B | 0.325 (5) | 0.777 (6) | 0.236 (3) | 0.132 (13)* | |
H3A | 0.273 (3) | 0.218 (4) | 0.403 (3) | 0.093 (10)* | |
H3B | 0.369 (4) | 0.237 (3) | 0.2981 (12) | 0.075 (8)* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Na1 | 0.0431 (4) | 0.0405 (4) | 0.0374 (4) | 0.0091 (3) | 0.0063 (3) | 0.0092 (3) |
S1 | 0.0500 (3) | 0.0312 (2) | 0.0276 (2) | 0.00480 (17) | 0.00090 (16) | 0.00630 (16) |
C5 | 0.0254 (7) | 0.0290 (7) | 0.0290 (7) | 0.0030 (5) | 0.0023 (5) | 0.0038 (6) |
C6 | 0.0583 (11) | 0.0297 (8) | 0.0456 (10) | −0.0008 (7) | 0.0112 (8) | −0.0009 (7) |
N1 | 0.0401 (7) | 0.0332 (7) | 0.0329 (7) | 0.0075 (5) | 0.0021 (5) | 0.0084 (5) |
N2 | 0.0387 (7) | 0.0473 (8) | 0.0337 (7) | 0.0082 (6) | 0.0030 (5) | 0.0142 (6) |
N3 | 0.0339 (7) | 0.0488 (8) | 0.0279 (6) | 0.0037 (6) | 0.0031 (5) | 0.0073 (6) |
N4 | 0.0310 (6) | 0.0313 (6) | 0.0281 (6) | 0.0023 (5) | 0.0032 (5) | 0.0026 (5) |
O1 | 0.0586 (7) | 0.0306 (6) | 0.0329 (6) | 0.0080 (5) | −0.0008 (5) | 0.0075 (5) |
O2 | 0.0584 (9) | 0.0804 (11) | 0.0600 (9) | −0.0048 (8) | −0.0025 (7) | 0.0407 (8) |
O3 | 0.0495 (7) | 0.0433 (7) | 0.0347 (6) | 0.0034 (6) | 0.0048 (5) | 0.0013 (5) |
Geometric parameters (Å, º) top
Na1—O1 | 2.4225 (14) | C6—H6B | 0.9600 |
Na1—O2 | 2.3353 (15) | C6—H6C | 0.9600 |
Na1—O3 | 2.4493 (14) | N1—N2 | 1.3566 (18) |
Na1—O1i | 2.4543 (13) | N2—N3 | 1.289 (2) |
Na1—O3ii | 2.4851 (14) | N3—N4 | 1.3485 (18) |
Na1—S1 | 3.0163 (8) | O1—Na1i | 2.4543 (13) |
Na1—Na1ii | 3.6215 (12) | O1—H1A | 0.822 (10) |
Na1—Na1i | 3.7073 (13) | O1—H1B | 0.822 (10) |
S1—C5 | 1.7133 (14) | O2—H2A | 0.822 (10) |
C5—N1 | 1.3391 (19) | O2—H2B | 0.814 (10) |
C5—N4 | 1.3513 (18) | O3—Na1ii | 2.4851 (14) |
C6—N4 | 1.450 (2) | O3—H3A | 0.813 (10) |
C6—H6A | 0.9600 | O3—H3B | 0.813 (10) |
| | | |
O2—Na1—O1 | 92.10 (5) | N1—C5—S1 | 127.98 (11) |
O2—Na1—O3 | 94.87 (6) | N4—C5—S1 | 125.65 (11) |
O1—Na1—O3 | 100.02 (5) | N4—C6—H6A | 109.5 |
O2—Na1—O1i | 172.45 (6) | N4—C6—H6B | 109.5 |
O1—Na1—O1i | 81.04 (5) | H6A—C6—H6B | 109.5 |
O3—Na1—O1i | 83.29 (5) | N4—C6—H6C | 109.5 |
O2—Na1—O3ii | 87.70 (5) | H6A—C6—H6C | 109.5 |
O1—Na1—O3ii | 174.40 (5) | H6B—C6—H6C | 109.5 |
O3—Na1—O3ii | 85.57 (5) | C5—N1—N2 | 106.93 (12) |
O1i—Na1—O3ii | 99.43 (5) | N3—N2—N1 | 110.70 (12) |
O2—Na1—S1 | 98.58 (5) | N2—N3—N4 | 106.60 (12) |
O1—Na1—S1 | 84.02 (3) | N3—N4—C5 | 109.41 (12) |
O3—Na1—S1 | 165.82 (4) | N3—N4—C6 | 121.45 (13) |
O1i—Na1—S1 | 83.94 (3) | C5—N4—C6 | 129.14 (13) |
O3ii—Na1—S1 | 90.47 (3) | Na1—O1—Na1i | 98.96 (4) |
O2—Na1—Na1ii | 91.71 (5) | Na1—O1—H1A | 104.6 (15) |
O1—Na1—Na1ii | 143.19 (4) | Na1i—O1—H1A | 129.1 (15) |
O3—Na1—Na1ii | 43.17 (3) | Na1—O1—H1B | 118.0 (15) |
O1i—Na1—Na1ii | 91.91 (4) | Na1i—O1—H1B | 97.4 (15) |
O3ii—Na1—Na1ii | 42.40 (3) | H1A—O1—H1B | 110 (2) |
S1—Na1—Na1ii | 131.41 (3) | Na1—O2—H2A | 119 (2) |
O2—Na1—Na1i | 132.86 (5) | Na1—O2—H2B | 134 (3) |
O1—Na1—Na1i | 40.84 (3) | H2A—O2—H2B | 102 (3) |
O3—Na1—Na1i | 92.08 (4) | Na1—O3—Na1ii | 94.43 (5) |
O1i—Na1—Na1i | 40.20 (3) | Na1—O3—H3A | 98 (2) |
O3ii—Na1—Na1i | 139.36 (4) | Na1ii—O3—H3A | 126 (2) |
S1—Na1—Na1i | 82.07 (2) | Na1—O3—H3B | 122.8 (18) |
Na1ii—Na1—Na1i | 123.04 (3) | Na1ii—O3—H3B | 111.3 (18) |
C5—S1—Na1 | 103.08 (5) | H3A—O3—H3B | 105 (3) |
N1—C5—N4 | 106.36 (12) | | |
| | | |
O2—Na1—S1—C5 | −145.34 (6) | N1—C5—N4—N3 | 0.44 (15) |
O1—Na1—S1—C5 | 123.42 (6) | S1—C5—N4—N3 | −179.45 (10) |
O3—Na1—S1—C5 | 16.00 (18) | N1—C5—N4—C6 | −179.67 (14) |
O1i—Na1—S1—C5 | 41.84 (6) | S1—C5—N4—C6 | 0.4 (2) |
O3ii—Na1—S1—C5 | −57.60 (6) | O2—Na1—O1—Na1i | 176.81 (6) |
Na1ii—Na1—S1—C5 | −45.36 (6) | O3—Na1—O1—Na1i | 81.49 (5) |
Na1i—Na1—S1—C5 | 82.31 (5) | O1i—Na1—O1—Na1i | 0.0 |
Na1—S1—C5—N1 | −25.60 (14) | S1—Na1—O1—Na1i | −84.78 (4) |
Na1—S1—C5—N4 | 154.27 (11) | Na1ii—Na1—O1—Na1i | 81.13 (7) |
N4—C5—N1—N2 | −0.34 (15) | O2—Na1—O3—Na1ii | 87.31 (5) |
S1—C5—N1—N2 | 179.54 (10) | O1—Na1—O3—Na1ii | −179.68 (5) |
C5—N1—N2—N3 | 0.13 (16) | O1i—Na1—O3—Na1ii | −100.06 (5) |
N1—N2—N3—N4 | 0.14 (16) | O3ii—Na1—O3—Na1ii | 0.0 |
N2—N3—N4—C5 | −0.37 (15) | S1—Na1—O3—Na1ii | −74.18 (17) |
N2—N3—N4—C6 | 179.73 (13) | Na1i—Na1—O3—Na1ii | −139.36 (4) |
Symmetry codes: (i) −x, −y+1, −z+1; (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 |
O2—H2A···S1iii | 0.82 (1) | 2.56 (1) | 3.3632 (16) | 166 (3) |
O2—H2B···N2iv | 0.81 (1) | 2.30 (2) | 3.084 (2) | 163 (4) |
O3—H3B···N3v | 0.81 (1) | 2.23 (1) | 3.0075 (18) | 162 (2) |
O3—H3A···S1i | 0.81 (1) | 2.75 (2) | 3.4769 (14) | 150 (3) |
O1—H1B···N1i | 0.82 (1) | 2.00 (1) | 2.8123 (18) | 171 (2) |
O1—H1A···S1vi | 0.82 (1) | 2.54 (1) | 3.3513 (12) | 169 (2) |
Symmetry codes: (i) −x, −y+1, −z+1; (iii) −x+1, −y+2, −z+1; (iv) x, y, z−1; (v) x, y−1, z−1; (vi) −x, −y+2, −z+1. |
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