Download citation
Download citation
link to html
The asymmetric unit of the title compound, (C7H8N4)2[CoCl4]·H2O, contains one [CoCl4]2- anion, two 5,7-dimethyl-1,2,4-triazolo[1,5-a]pyrimidinium cations monoprotonated at the N atom at position 3 and one uncoordinated water mol­ecule. Hydrogen bonds define infinite chains along the a axis, which link together all residues.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536805024633/ya6255sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536805024633/ya6255Isup2.hkl
Contains datablock I

CCDC reference: 284013

Key indicators

  • Single-crystal X-ray study
  • T = 298 K
  • Mean [sigma](C-C) = 0.003 Å
  • R factor = 0.031
  • wR factor = 0.080
  • Data-to-parameter ratio = 18.5

checkCIF/PLATON results

No syntax errors found



Alert level C PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT062_ALERT_4_C Rescale T(min) & T(max) by ..................... 0.98 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for Co PLAT431_ALERT_2_C Short Inter HL..A Contact Cl1 .. N8B .. 3.29 Ang. PLAT431_ALERT_2_C Short Inter HL..A Contact Cl2 .. N8A .. 3.24 Ang. PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 2 PLAT731_ALERT_1_C Bond Calc 0.845(19), Rep 0.844(9) ...... 2.11 su-Rat O1W -H11W 1.555 1.555 PLAT735_ALERT_1_C D-H Calc 0.845(19), Rep 0.844(9) ...... 2.11 su-Rat O1W -H11W 1.555 1.555
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 8 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 3 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

Computing details top

Data collection: SMART (Bruker, 1999); cell refinement: SAINT (Bruker, 1999); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: Xtal_GX (Hall & du Boulay, 1997); software used to prepare material for publication: SHELXL97.

5,7-dimethyl-1,2,4-triazolo[1,5-a]pyrimidinium tetrachlorocobaltate(II) monohydrate top
Crystal data top
2C7H9N4+·Cl4Co2·H2OZ = 2
Mr = 517.11F(000) = 526
Triclinic, P1Dx = 1.600 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 7.6369 (4) ÅCell parameters from 5772 reflections
b = 8.5190 (4) Åθ = 2.2–27.2°
c = 18.2777 (9) ŵ = 1.32 mm1
α = 84.952 (1)°T = 298 K
β = 84.505 (1)°Prism, blue
γ = 65.275 (1)°0.46 × 0.29 × 0.23 mm
V = 1073.64 (9) Å3
Data collection top
Bruker SMART APEX CCD
diffractometer
4866 independent reflections
Radiation source: fine-focus sealed tube4217 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.019
Detector resolution: 8.26 pixels mm-1θmax = 28.3°, θmin = 2.2°
φ and ω scansh = 910
Absorption correction: multi-scan
(SADABS; Bruker, 1999)
k = 1111
Tmin = 0.668, Tmax = 0.751l = 2423
12624 measured reflections
Refinement top
Refinement on F2Primary atom site location: heavy-atom method
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.031Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.080H atoms treated by a mixture of independent and constrained refinement
S = 1.04 w = 1/[σ2(Fo2) + (0.04P)2 + 0.25P]
where P = (Fo2 + 2Fc2)/3
4866 reflections(Δ/σ)max = 0.002
263 parametersΔρmax = 0.45 e Å3
3 restraintsΔρmin = 0.36 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*/Ueq
Co0.11422 (3)0.44963 (3)0.248561 (13)0.03963 (9)
Cl10.00141 (7)0.64882 (6)0.33725 (3)0.05152 (13)
Cl20.34565 (7)0.48632 (7)0.17064 (3)0.05223 (13)
Cl30.12146 (8)0.46295 (8)0.17920 (3)0.06222 (15)
Cl40.25025 (11)0.19090 (7)0.31175 (3)0.06899 (18)
N1A0.3772 (2)0.7362 (2)0.00403 (9)0.0445 (4)
C2A0.2741 (3)0.6835 (2)0.03184 (11)0.0455 (4)
H2A0.32270.61780.07300.055*
N3A0.0906 (2)0.73306 (19)0.00317 (9)0.0424 (3)
H3A0.00170.71130.01960.051*
C3aA0.0734 (2)0.8231 (2)0.05597 (10)0.0375 (4)
N4A0.0789 (2)0.89762 (19)0.10141 (9)0.0420 (3)
C5A0.0487 (3)0.9754 (2)0.15607 (11)0.0440 (4)
C51A0.2146 (3)1.0602 (3)0.21017 (13)0.0600 (6)
H51A0.32981.12400.18460.072*
H52A0.18771.13770.23760.072*
H53A0.23280.97350.24330.072*
C6A0.1319 (3)0.9785 (2)0.16388 (11)0.0467 (4)
H6A0.14601.03380.20310.056*
C7A0.2853 (3)0.9025 (2)0.11524 (11)0.0434 (4)
C71A0.4817 (3)0.8951 (3)0.11745 (14)0.0605 (6)
H71A0.57170.77660.12460.073*
H72A0.48440.95970.15740.073*
H73A0.51670.94340.07190.073*
N8A0.2486 (2)0.82536 (18)0.05973 (8)0.0377 (3)
N1B0.4223 (3)0.2049 (2)0.54414 (10)0.0509 (4)
C2B0.3349 (3)0.2344 (3)0.48328 (11)0.0518 (5)
H2B0.34060.14630.45520.062*
N3B0.2361 (2)0.4043 (2)0.46483 (9)0.0507 (4)
H3B0.16990.44800.42690.061*
C3aB0.2623 (3)0.4920 (2)0.51784 (10)0.0434 (4)
N4B0.1948 (3)0.6608 (2)0.52371 (9)0.0516 (4)
C5B0.2455 (3)0.7079 (3)0.58343 (11)0.0514 (5)
C51B0.1717 (4)0.8983 (3)0.59242 (15)0.0736 (7)
H51B0.05650.93670.62460.088*
H52B0.26900.92140.61300.088*
H53B0.14350.95900.54520.088*
C6B0.3597 (3)0.5869 (3)0.63552 (11)0.0507 (5)
H6B0.39120.62640.67600.061*
C7B0.4265 (3)0.4134 (3)0.62791 (11)0.0461 (4)
C71B0.5435 (4)0.2725 (3)0.67934 (13)0.0646 (6)
H71B0.56000.32100.72230.078*
H72B0.47910.19790.69360.078*
H73B0.66760.20710.65540.078*
N8B0.3753 (2)0.37010 (19)0.56583 (8)0.0407 (3)
O1W0.2132 (2)0.3126 (2)0.04297 (9)0.0669 (5)
H11W0.324 (2)0.298 (3)0.0241 (12)0.080*
H12W0.195 (3)0.359 (3)0.0834 (8)0.080*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Co0.04355 (15)0.03955 (14)0.03598 (14)0.01714 (11)0.00103 (10)0.00496 (10)
Cl10.0591 (3)0.0440 (3)0.0459 (3)0.0150 (2)0.0016 (2)0.0120 (2)
Cl20.0497 (3)0.0594 (3)0.0497 (3)0.0261 (2)0.0065 (2)0.0059 (2)
Cl30.0493 (3)0.0757 (4)0.0647 (3)0.0248 (3)0.0104 (2)0.0168 (3)
Cl40.1134 (5)0.0401 (3)0.0502 (3)0.0262 (3)0.0190 (3)0.0007 (2)
N1A0.0373 (8)0.0475 (9)0.0453 (9)0.0138 (7)0.0028 (7)0.0042 (7)
C2A0.0426 (10)0.0467 (10)0.0450 (10)0.0154 (8)0.0033 (8)0.0064 (8)
N3A0.0409 (8)0.0438 (8)0.0457 (9)0.0188 (7)0.0069 (7)0.0082 (7)
C3aA0.0376 (9)0.0340 (8)0.0432 (9)0.0164 (7)0.0089 (7)0.0014 (7)
N4A0.0374 (8)0.0394 (8)0.0487 (9)0.0149 (6)0.0026 (6)0.0044 (7)
C5A0.0471 (10)0.0361 (9)0.0458 (10)0.0139 (8)0.0050 (8)0.0027 (8)
C51A0.0601 (13)0.0608 (13)0.0573 (13)0.0229 (11)0.0079 (10)0.0176 (10)
C6A0.0533 (11)0.0434 (10)0.0457 (10)0.0196 (9)0.0112 (9)0.0070 (8)
C7A0.0443 (10)0.0400 (9)0.0493 (10)0.0188 (8)0.0150 (8)0.0003 (8)
C71A0.0490 (12)0.0706 (14)0.0698 (15)0.0289 (11)0.0161 (10)0.0093 (12)
N8A0.0349 (7)0.0369 (7)0.0407 (8)0.0140 (6)0.0058 (6)0.0009 (6)
N1B0.0606 (10)0.0428 (9)0.0512 (10)0.0217 (8)0.0021 (8)0.0115 (7)
C2B0.0609 (13)0.0516 (12)0.0495 (11)0.0285 (10)0.0001 (9)0.0127 (9)
N3B0.0585 (10)0.0572 (10)0.0401 (9)0.0267 (8)0.0042 (7)0.0066 (7)
C3aB0.0470 (10)0.0491 (10)0.0363 (9)0.0232 (9)0.0058 (8)0.0066 (8)
N4B0.0613 (11)0.0446 (9)0.0460 (9)0.0201 (8)0.0029 (8)0.0032 (7)
C5B0.0618 (13)0.0450 (11)0.0489 (11)0.0253 (10)0.0120 (9)0.0104 (9)
C51B0.101 (2)0.0473 (12)0.0685 (16)0.0273 (13)0.0049 (14)0.0127 (11)
C6B0.0595 (12)0.0528 (11)0.0453 (11)0.0279 (10)0.0039 (9)0.0139 (9)
C7B0.0481 (11)0.0501 (11)0.0429 (10)0.0230 (9)0.0001 (8)0.0068 (8)
C71B0.0742 (15)0.0571 (13)0.0612 (14)0.0215 (11)0.0230 (12)0.0048 (11)
N8B0.0442 (8)0.0394 (8)0.0404 (8)0.0192 (7)0.0026 (6)0.0072 (6)
O1W0.0530 (9)0.1006 (13)0.0621 (10)0.0426 (9)0.0058 (7)0.0345 (9)
Geometric parameters (Å, º) top
Co—Cl12.2898 (5)C71A—H73A0.9600
Co—Cl22.2697 (5)N1B—C2B1.303 (3)
Co—Cl32.2583 (6)N1B—N8B1.383 (2)
Co—Cl42.2666 (6)C2B—N3B1.352 (3)
N1A—C2A1.303 (2)C2B—H2B0.9300
N1A—N8A1.378 (2)N3B—C3aB1.351 (2)
C2A—N3A1.349 (2)N3B—H3B0.8600
C2A—H2A0.9300C3aB—N4B1.319 (2)
N3A—C3aA1.345 (2)C3aB—N8B1.352 (2)
N3A—H3A0.8600N4B—C5B1.338 (3)
C3aA—N4A1.317 (2)C5B—C6B1.402 (3)
C3aA—N8A1.355 (2)C5B—C51B1.497 (3)
N4A—C5A1.334 (2)C51B—H51B0.9600
C5A—C6A1.411 (3)C51B—H52B0.9600
C5A—C51A1.492 (3)C51B—H53B0.9600
C51A—H51A0.9600C6B—C7B1.363 (3)
C51A—H52A0.9600C6B—H6B0.9300
C51A—H53A0.9600C7B—N8B1.362 (2)
C6A—C7A1.360 (3)C7B—C71B1.479 (3)
C6A—H6A0.9300C71B—H71B0.9600
C7A—N8A1.365 (2)C71B—H72B0.9600
C7A—C71A1.479 (3)C71B—H73B0.9600
C71A—H71A0.9600O1W—H11W0.844 (9)
C71A—H72A0.9600O1W—H12W0.843 (9)
Cl3—Co—Cl4112.31 (3)C3aA—N8A—N1A111.43 (14)
Cl3—Co—Cl2107.13 (2)C7A—N8A—N1A127.10 (15)
Cl4—Co—Cl2108.47 (3)C2B—N1B—N8B102.66 (16)
Cl3—Co—Cl1112.49 (2)N1B—C2B—N3B113.79 (18)
Cl4—Co—Cl1104.59 (2)N1B—C2B—H2B122.9
Cl2—Co—Cl1111.86 (2)N3B—C2B—H2B123.3
C2A—N1A—N8A102.88 (14)C3aB—N3B—C2B106.35 (17)
N1A—C2A—N3A113.40 (17)C3aB—N3B—H3B126.8
N1A—C2A—H2A123.2C2B—N3B—H3B126.8
N3A—C2A—H2A123.4N4B—C3aB—N3B128.83 (19)
C3aA—N3A—C2A106.80 (15)N4B—C3aB—N8B125.44 (17)
C3aA—N3A—H3A126.6N3B—C3aB—N8B105.73 (16)
C2A—N3A—H3A126.6C3aB—N4B—C5B114.52 (18)
N4A—C3aA—N3A128.99 (16)N4B—C5B—C6B122.37 (18)
N4A—C3aA—N8A125.53 (16)N4B—C5B—C51B116.4 (2)
N3A—C3aA—N8A105.48 (15)C6B—C5B—C51B121.3 (2)
C3aA—N4A—C5A114.64 (16)C5B—C51B—H51B110.0
N4A—C5A—C6A122.39 (17)C5B—C51B—H52B109.0
N4A—C5A—C51A117.38 (18)H51B—C51B—H52B109.5
C6A—C5A—C51A120.23 (18)C5B—C51B—H53B109.4
C5A—C51A—H51A109.7H51B—C51B—H53B109.5
C5A—C51A—H52A109.2H52B—C51B—H53B109.5
H51A—C51A—H52A109.5C7B—C6B—C5B121.60 (19)
C5A—C51A—H53A109.5C7B—C6B—H6B119.4
H51A—C51A—H53A109.5C5B—C6B—H6B119.0
H52A—C51A—H53A109.5N8B—C7B—C6B114.45 (18)
C7A—C6A—C5A121.38 (17)N8B—C7B—C71B118.40 (18)
C7A—C6A—H6A119.4C6B—C7B—C71B127.14 (19)
C5A—C6A—H6A119.2C7B—C71B—H71B109.6
C6A—C7A—N8A114.60 (16)C7B—C71B—H72B109.6
C6A—C7A—C71A126.78 (18)H71B—C71B—H72B109.5
N8A—C7A—C71A118.62 (18)C7B—C71B—H73B109.3
C7A—C71A—H71A109.1H71B—C71B—H73B109.5
C7A—C71A—H72A109.5H72B—C71B—H73B109.5
H71A—C71A—H72A109.5C3aB—N8B—C7B121.59 (16)
C7A—C71A—H73A109.8C3aB—N8B—N1B111.47 (15)
H71A—C71A—H73A109.5C7B—N8B—N1B126.92 (16)
H72A—C71A—H73A109.5H11W—O1W—H12W108.6 (15)
C3aA—N8A—C7A121.41 (16)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N3A—H3A···O1Wi0.861.832.681 (2)171
N3B—H3B···Cl10.862.313.1325 (18)160
O1W—H11W···N1Aii0.84 (1)2.19 (1)3.026 (2)169 (2)
O1W—H12W···Cl20.84 (1)2.59 (2)3.3122 (15)144 (2)
Symmetry codes: (i) x, y+1, z; (ii) x+1, y+1, z.
 

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