Buy article online - an online subscription or single-article purchase is required to access this article.
Download citation
Download citation
link to html
The structure of the title compound, C7H8N4S·1.75H2O, is similar to that of pyridine-2-carb­aldehyde thio­semicarbazone dihydrate [Huang (1993). J. X. Univ. (Nat. Sci.), 32, 741-744], except for the disorder in a water mol­ecule and presence of another water mol­ecule at special position (1/2, 3/4, 1/8).

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S160053680302511X/ci6283sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S160053680302511X/ci6283Isup2.hkl
Contains datablock I

CCDC reference: 190349

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](C-C) = 0.003 Å
  • R factor = 0.040
  • wR factor = 0.095
  • Data-to-parameter ratio = 15.0

checkCIF/PLATON results

No syntax errors found



Alert level B PLAT417_ALERT_2_B Short Inter D-H..H-D H1O1 .. H1O3 = 1.24 Ang.
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 ............ 0.25 Ratio PLAT301_ALERT_3_C Main Residue Disorder ......................... 3.00 Perc. PLAT417_ALERT_2_C Short Inter D-H..H-D H1O1 .. H1O2 = 2.10 Ang. PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 5
0 ALERT level A = In general: serious problem 1 ALERT level B = Potentially serious problem 6 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 2 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

Computing details top

Data collection: XSCANS (Siemens, 1994); cell refinement: XSCANS; data reduction: XSCANS; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Siemens, 1994); software used to prepare material for publication: SHELXTL.

Pyridine-2-carbaldehyde thiosemicarbazone 1.75-hydrate top
Crystal data top
C7H8N4S·1.75H2ODx = 1.356 Mg m3
Mr = 211.76Mo Kα radiation, λ = 0.71073 Å
Tetragonal, I41/aCell parameters from 39 reflections
Hall symbol: -I 4adθ = 2.8–14.9°
a = 13.676 (1) ŵ = 0.29 mm1
c = 22.192 (3) ÅT = 293 K
V = 4150.6 (7) Å3Plate, yellow
Z = 160.48 × 0.48 × 0.44 mm
F(000) = 1784
Data collection top
Siemens P4
diffractometer
1437 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tubeRint = 0.020
Graphite monochromatorθmax = 26.5°, θmin = 1.8°
θ/2θ scansh = 017
Absorption correction: ψ scan
(North et al., 1968)
k = 017
Tmin = 0.831, Tmax = 0.880l = 127
2473 measured reflections3 standard reflections every 97 reflections
2158 independent reflections intensity decay: 2.8%
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.040Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.095H atoms treated by a mixture of independent and constrained refinement
S = 0.93 w = 1/[σ2(Fo2) + (0.0502P)2]
where P = (Fo2 + 2Fc2)/3
2158 reflections(Δ/σ)max = 0.001
144 parametersΔρmax = 0.13 e Å3
10 restraintsΔρmin = 0.18 e Å3
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
xyzUiso*/UeqOcc. (<1)
S0.35971 (4)0.42035 (4)0.10319 (2)0.05532 (19)
N10.15439 (11)0.36195 (11)0.04923 (7)0.0472 (4)
N20.10107 (11)0.39167 (10)0.03125 (7)0.0418 (4)
N30.17588 (11)0.40563 (11)0.07153 (7)0.0437 (4)
H3N0.16350.40940.10950.052*
N40.28360 (11)0.41412 (11)0.00676 (7)0.0498 (4)
H4A0.23480.40970.03100.060*
H4B0.34200.41900.02080.060*
C10.23631 (15)0.34362 (15)0.01825 (9)0.0560 (5)
H10.29460.33760.03960.067*
C20.23917 (16)0.33317 (15)0.04301 (10)0.0594 (6)
H20.29780.32020.06270.071*
C30.15371 (16)0.34223 (14)0.07480 (10)0.0570 (6)
H30.15380.33630.11650.068*
C40.06778 (15)0.36019 (13)0.04457 (8)0.0476 (5)
H40.00900.36590.06540.057*
C50.07077 (13)0.36951 (12)0.01752 (8)0.0406 (4)
C60.01594 (14)0.38719 (13)0.05404 (8)0.0448 (5)
H60.00880.39550.09540.054*
C70.26893 (13)0.41344 (13)0.05173 (8)0.0410 (4)
O10.51492 (15)0.58711 (17)0.05087 (10)0.0968 (6)
O20.4778 (5)0.2231 (5)0.04034 (19)0.1060 (18)0.50
O30.50000.75000.12500.0993 (12)
H1O10.505 (2)0.6278 (18)0.0759 (13)0.149*
H2O10.478 (2)0.5406 (16)0.0536 (15)0.149*
H1O20.489 (5)0.190 (4)0.0100 (15)0.149*0.50
H2O20.525 (4)0.212 (6)0.063 (2)0.149*0.50
H1O30.481 (6)0.795 (3)0.1038 (5)0.149*0.50
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
S0.0492 (3)0.0736 (4)0.0432 (3)0.0001 (3)0.0060 (2)0.0002 (3)
N10.0435 (9)0.0515 (10)0.0468 (9)0.0004 (8)0.0011 (8)0.0015 (8)
N20.0441 (9)0.0402 (9)0.0410 (9)0.0002 (7)0.0028 (7)0.0007 (7)
N30.0450 (9)0.0507 (10)0.0355 (8)0.0008 (7)0.0000 (7)0.0006 (7)
N40.0438 (10)0.0650 (11)0.0405 (9)0.0029 (8)0.0000 (7)0.0011 (8)
C10.0442 (12)0.0598 (14)0.0638 (14)0.0011 (10)0.0013 (10)0.0049 (11)
C20.0541 (13)0.0563 (14)0.0678 (15)0.0016 (11)0.0155 (12)0.0077 (11)
C30.0752 (16)0.0503 (13)0.0454 (12)0.0001 (11)0.0109 (11)0.0051 (10)
C40.0540 (12)0.0440 (11)0.0447 (11)0.0018 (9)0.0032 (9)0.0019 (9)
C50.0442 (11)0.0339 (10)0.0436 (10)0.0008 (8)0.0005 (8)0.0012 (8)
C60.0491 (12)0.0465 (11)0.0390 (10)0.0004 (9)0.0003 (9)0.0006 (8)
C70.0474 (11)0.0353 (10)0.0403 (10)0.0019 (8)0.0016 (9)0.0013 (8)
O10.0775 (13)0.1067 (17)0.1063 (16)0.0238 (12)0.0294 (11)0.0172 (12)
O20.100 (5)0.113 (6)0.105 (3)0.025 (3)0.017 (3)0.028 (3)
O30.1042 (18)0.1042 (18)0.089 (3)0.0000.0000.000
Geometric parameters (Å, º) top
S—C71.6895 (18)C2—H20.93
N1—C11.338 (2)C3—C41.375 (3)
N1—C51.347 (2)C3—H30.93
N2—C61.271 (2)C4—C51.384 (3)
N2—N31.372 (2)C4—H40.93
N3—C71.351 (2)C5—C61.457 (3)
N3—H3N0.86C6—H60.93
N4—C71.314 (2)O1—H1O10.80 (3)
N4—H4A0.86O1—H2O10.81 (2)
N4—H4B0.86O2—O2i0.953 (10)
C1—C21.368 (3)O2—H1O20.83 (4)
C1—H10.93O2—H2O20.83 (5)
C2—C31.371 (3)O3—H1O30.82 (4)
C1—N1—C5117.18 (17)C3—C4—C5118.47 (19)
C6—N2—N3115.51 (15)C3—C4—H4120.8
C7—N3—N2120.11 (15)C5—C4—H4120.8
C7—N3—H3N119.9N1—C5—C4122.56 (18)
N2—N3—H3N119.9N1—C5—C6114.42 (16)
C7—N4—H4A120.0C4—C5—C6123.02 (18)
C7—N4—H4B120.0N2—C6—C5122.18 (17)
H4A—N4—H4B120.0N2—C6—H6118.9
N1—C1—C2123.7 (2)C5—C6—H6118.9
N1—C1—H1118.2N4—C7—N3117.77 (16)
C2—C1—H1118.2N4—C7—S123.74 (15)
C1—C2—C3118.5 (2)N3—C7—S118.48 (14)
C1—C2—H2120.7H1O1—O1—H2O1113 (2)
C3—C2—H2120.7O2i—O2—H1O2108 (5)
C2—C3—C4119.59 (19)O2i—O2—H2O270 (6)
C2—C3—H3120.2H1O2—O2—H2O2104 (2)
C4—C3—H3120.2
C6—N2—N3—C7178.63 (16)C3—C4—C5—N10.2 (3)
C5—N1—C1—C20.5 (3)C3—C4—C5—C6179.12 (17)
N1—C1—C2—C30.2 (3)N3—N2—C6—C5178.00 (15)
C1—C2—C3—C40.8 (3)N1—C5—C6—N2176.72 (16)
C2—C3—C4—C50.6 (3)C4—C5—C6—N22.6 (3)
C1—N1—C5—C40.8 (3)N2—N3—C7—N44.7 (2)
C1—N1—C5—C6178.61 (17)N2—N3—C7—S174.56 (12)
Symmetry code: (i) x+1, y+1/2, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N4—H4A···N20.862.312.653 (2)104
O1—H1O1···O30.80 (3)2.00 (3)2.777 (2)166 (3)
O1—H2O1···S0.81 (2)2.56 (3)3.325 (2)158 (3)
N3—H3N···N1ii0.862.152.998 (2)171
O3—H1O3···O1iii0.82 (4)2.00 (3)2.777 (2)160 (9)
N4—H4A···Siv0.862.733.488 (2)148
N4—H4B···O1v0.862.072.924 (2)173
O2—H1O2···O1vi0.83 (4)1.98 (5)2.796 (6)168 (6)
O2—H2O2···Si0.83 (5)2.56 (7)3.277 (7)145 (7)
Symmetry codes: (i) x+1, y+1/2, z; (ii) y1/4, x+1/4, z+1/4; (iii) x+1, y+3/2, z; (iv) y1/4, x+3/4, z1/4; (v) x+1, y+1, z; (vi) x, y1/2, z.
 

Subscribe to Acta Crystallographica Section E: Crystallographic Communications

The full text of this article is available to subscribers to the journal.

If you have already registered and are using a computer listed in your registration details, please email support@iucr.org for assistance.

Buy online

You may purchase this article in PDF and/or HTML formats. For purchasers in the European Community who do not have a VAT number, VAT will be added at the local rate. Payments to the IUCr are handled by WorldPay, who will accept payment by credit card in several currencies. To purchase the article, please complete the form below (fields marked * are required), and then click on `Continue'.
E-mail address* 
Repeat e-mail address* 
(for error checking) 

Format*   PDF (US $40)
   HTML (US $40)
   PDF+HTML (US $50)
In order for VAT to be shown for your country javascript needs to be enabled.

VAT number 
(non-UK EC countries only) 
Country* 
 

Terms and conditions of use
Contact us

Follow Acta Cryst. E
Sign up for e-alerts
Follow Acta Cryst. on Twitter
Follow us on facebook
Sign up for RSS feeds