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
CCDC reference: 284013
Key indicators
- Single-crystal X-ray study
- T = 298 K
- Mean (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
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−·H2O | Z = 2 |
Mr = 517.11 | F(000) = 526 |
Triclinic, P1 | Dx = 1.600 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71073 Å |
a = 7.6369 (4) Å | Cell parameters from 5772 reflections |
b = 8.5190 (4) Å | θ = 2.2–27.2° |
c = 18.2777 (9) Å | µ = 1.32 mm−1 |
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 tube | 4217 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.019 |
Detector resolution: 8.26 pixels mm-1 | θmax = 28.3°, θmin = 2.2° |
φ and ω scans | h = −9→10 |
Absorption correction: multi-scan (SADABS; Bruker, 1999) | k = −11→11 |
Tmin = 0.668, Tmax = 0.751 | l = −24→23 |
12624 measured reflections | |
Refinement top
Refinement on F2 | Primary atom site location: heavy-atom method |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.031 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.080 | H 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 parameters | Δρmax = 0.45 e Å−3 |
3 restraints | Δρmin = −0.36 e Å−3 |
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 | |
Co | 0.11422 (3) | 0.44963 (3) | 0.248561 (13) | 0.03963 (9) | |
Cl1 | 0.00141 (7) | 0.64882 (6) | 0.33725 (3) | 0.05152 (13) | |
Cl2 | 0.34565 (7) | 0.48632 (7) | 0.17064 (3) | 0.05223 (13) | |
Cl3 | −0.12146 (8) | 0.46295 (8) | 0.17920 (3) | 0.06222 (15) | |
Cl4 | 0.25025 (11) | 0.19090 (7) | 0.31175 (3) | 0.06899 (18) | |
N1A | 0.3772 (2) | 0.7362 (2) | 0.00403 (9) | 0.0445 (4) | |
C2A | 0.2741 (3) | 0.6835 (2) | −0.03184 (11) | 0.0455 (4) | |
H2A | 0.3227 | 0.6178 | −0.0730 | 0.055* | |
N3A | 0.0906 (2) | 0.73306 (19) | −0.00317 (9) | 0.0424 (3) | |
H3A | 0.0017 | 0.7113 | −0.0196 | 0.051* | |
C3aA | 0.0734 (2) | 0.8231 (2) | 0.05597 (10) | 0.0375 (4) | |
N4A | −0.0789 (2) | 0.89762 (19) | 0.10141 (9) | 0.0420 (3) | |
C5A | −0.0487 (3) | 0.9754 (2) | 0.15607 (11) | 0.0440 (4) | |
C51A | −0.2146 (3) | 1.0602 (3) | 0.21017 (13) | 0.0600 (6) | |
H51A | −0.3298 | 1.1240 | 0.1846 | 0.072* | |
H52A | −0.1877 | 1.1377 | 0.2376 | 0.072* | |
H53A | −0.2328 | 0.9735 | 0.2433 | 0.072* | |
C6A | 0.1319 (3) | 0.9785 (2) | 0.16388 (11) | 0.0467 (4) | |
H6A | 0.1460 | 1.0338 | 0.2031 | 0.056* | |
C7A | 0.2853 (3) | 0.9025 (2) | 0.11524 (11) | 0.0434 (4) | |
C71A | 0.4817 (3) | 0.8951 (3) | 0.11745 (14) | 0.0605 (6) | |
H71A | 0.5717 | 0.7766 | 0.1246 | 0.073* | |
H72A | 0.4844 | 0.9597 | 0.1574 | 0.073* | |
H73A | 0.5167 | 0.9434 | 0.0719 | 0.073* | |
N8A | 0.2486 (2) | 0.82536 (18) | 0.05973 (8) | 0.0377 (3) | |
N1B | 0.4223 (3) | 0.2049 (2) | 0.54414 (10) | 0.0509 (4) | |
C2B | 0.3349 (3) | 0.2344 (3) | 0.48328 (11) | 0.0518 (5) | |
H2B | 0.3406 | 0.1463 | 0.4552 | 0.062* | |
N3B | 0.2361 (2) | 0.4043 (2) | 0.46483 (9) | 0.0507 (4) | |
H3B | 0.1699 | 0.4480 | 0.4269 | 0.061* | |
C3aB | 0.2623 (3) | 0.4920 (2) | 0.51784 (10) | 0.0434 (4) | |
N4B | 0.1948 (3) | 0.6608 (2) | 0.52371 (9) | 0.0516 (4) | |
C5B | 0.2455 (3) | 0.7079 (3) | 0.58343 (11) | 0.0514 (5) | |
C51B | 0.1717 (4) | 0.8983 (3) | 0.59242 (15) | 0.0736 (7) | |
H51B | 0.0565 | 0.9367 | 0.6246 | 0.088* | |
H52B | 0.2690 | 0.9214 | 0.6130 | 0.088* | |
H53B | 0.1435 | 0.9590 | 0.5452 | 0.088* | |
C6B | 0.3597 (3) | 0.5869 (3) | 0.63552 (11) | 0.0507 (5) | |
H6B | 0.3912 | 0.6264 | 0.6760 | 0.061* | |
C7B | 0.4265 (3) | 0.4134 (3) | 0.62791 (11) | 0.0461 (4) | |
C71B | 0.5435 (4) | 0.2725 (3) | 0.67934 (13) | 0.0646 (6) | |
H71B | 0.5600 | 0.3210 | 0.7223 | 0.078* | |
H72B | 0.4791 | 0.1979 | 0.6936 | 0.078* | |
H73B | 0.6676 | 0.2071 | 0.6554 | 0.078* | |
N8B | 0.3753 (2) | 0.37010 (19) | 0.56583 (8) | 0.0407 (3) | |
O1W | 0.2132 (2) | 0.3126 (2) | 0.04297 (9) | 0.0669 (5) | |
H11W | 0.324 (2) | 0.298 (3) | 0.0241 (12) | 0.080* | |
H12W | 0.195 (3) | 0.359 (3) | 0.0834 (8) | 0.080* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Co | 0.04355 (15) | 0.03955 (14) | 0.03598 (14) | −0.01714 (11) | −0.00103 (10) | −0.00496 (10) |
Cl1 | 0.0591 (3) | 0.0440 (3) | 0.0459 (3) | −0.0150 (2) | 0.0016 (2) | −0.0120 (2) |
Cl2 | 0.0497 (3) | 0.0594 (3) | 0.0497 (3) | −0.0261 (2) | 0.0065 (2) | −0.0059 (2) |
Cl3 | 0.0493 (3) | 0.0757 (4) | 0.0647 (3) | −0.0248 (3) | −0.0104 (2) | −0.0168 (3) |
Cl4 | 0.1134 (5) | 0.0401 (3) | 0.0502 (3) | −0.0262 (3) | −0.0190 (3) | 0.0007 (2) |
N1A | 0.0373 (8) | 0.0475 (9) | 0.0453 (9) | −0.0138 (7) | −0.0028 (7) | −0.0042 (7) |
C2A | 0.0426 (10) | 0.0467 (10) | 0.0450 (10) | −0.0154 (8) | −0.0033 (8) | −0.0064 (8) |
N3A | 0.0409 (8) | 0.0438 (8) | 0.0457 (9) | −0.0188 (7) | −0.0069 (7) | −0.0082 (7) |
C3aA | 0.0376 (9) | 0.0340 (8) | 0.0432 (9) | −0.0164 (7) | −0.0089 (7) | 0.0014 (7) |
N4A | 0.0374 (8) | 0.0394 (8) | 0.0487 (9) | −0.0149 (6) | −0.0026 (6) | −0.0044 (7) |
C5A | 0.0471 (10) | 0.0361 (9) | 0.0458 (10) | −0.0139 (8) | −0.0050 (8) | −0.0027 (8) |
C51A | 0.0601 (13) | 0.0608 (13) | 0.0573 (13) | −0.0229 (11) | 0.0079 (10) | −0.0176 (10) |
C6A | 0.0533 (11) | 0.0434 (10) | 0.0457 (10) | −0.0196 (9) | −0.0112 (9) | −0.0070 (8) |
C7A | 0.0443 (10) | 0.0400 (9) | 0.0493 (10) | −0.0188 (8) | −0.0150 (8) | 0.0003 (8) |
C71A | 0.0490 (12) | 0.0706 (14) | 0.0698 (15) | −0.0289 (11) | −0.0161 (10) | −0.0093 (12) |
N8A | 0.0349 (7) | 0.0369 (7) | 0.0407 (8) | −0.0140 (6) | −0.0058 (6) | −0.0009 (6) |
N1B | 0.0606 (10) | 0.0428 (9) | 0.0512 (10) | −0.0217 (8) | −0.0021 (8) | −0.0115 (7) |
C2B | 0.0609 (13) | 0.0516 (12) | 0.0495 (11) | −0.0285 (10) | 0.0001 (9) | −0.0127 (9) |
N3B | 0.0585 (10) | 0.0572 (10) | 0.0401 (9) | −0.0267 (8) | −0.0042 (7) | −0.0066 (7) |
C3aB | 0.0470 (10) | 0.0491 (10) | 0.0363 (9) | −0.0232 (9) | 0.0058 (8) | −0.0066 (8) |
N4B | 0.0613 (11) | 0.0446 (9) | 0.0460 (9) | −0.0201 (8) | 0.0029 (8) | −0.0032 (7) |
C5B | 0.0618 (13) | 0.0450 (11) | 0.0489 (11) | −0.0253 (10) | 0.0120 (9) | −0.0104 (9) |
C51B | 0.101 (2) | 0.0473 (12) | 0.0685 (16) | −0.0273 (13) | 0.0049 (14) | −0.0127 (11) |
C6B | 0.0595 (12) | 0.0528 (11) | 0.0453 (11) | −0.0279 (10) | 0.0039 (9) | −0.0139 (9) |
C7B | 0.0481 (11) | 0.0501 (11) | 0.0429 (10) | −0.0230 (9) | 0.0001 (8) | −0.0068 (8) |
C71B | 0.0742 (15) | 0.0571 (13) | 0.0612 (14) | −0.0215 (11) | −0.0230 (12) | −0.0048 (11) |
N8B | 0.0442 (8) | 0.0394 (8) | 0.0404 (8) | −0.0192 (7) | 0.0026 (6) | −0.0072 (6) |
O1W | 0.0530 (9) | 0.1006 (13) | 0.0621 (10) | −0.0426 (9) | 0.0058 (7) | −0.0345 (9) |
Geometric parameters (Å, º) top
Co—Cl1 | 2.2898 (5) | C71A—H73A | 0.9600 |
Co—Cl2 | 2.2697 (5) | N1B—C2B | 1.303 (3) |
Co—Cl3 | 2.2583 (6) | N1B—N8B | 1.383 (2) |
Co—Cl4 | 2.2666 (6) | C2B—N3B | 1.352 (3) |
N1A—C2A | 1.303 (2) | C2B—H2B | 0.9300 |
N1A—N8A | 1.378 (2) | N3B—C3aB | 1.351 (2) |
C2A—N3A | 1.349 (2) | N3B—H3B | 0.8600 |
C2A—H2A | 0.9300 | C3aB—N4B | 1.319 (2) |
N3A—C3aA | 1.345 (2) | C3aB—N8B | 1.352 (2) |
N3A—H3A | 0.8600 | N4B—C5B | 1.338 (3) |
C3aA—N4A | 1.317 (2) | C5B—C6B | 1.402 (3) |
C3aA—N8A | 1.355 (2) | C5B—C51B | 1.497 (3) |
N4A—C5A | 1.334 (2) | C51B—H51B | 0.9600 |
C5A—C6A | 1.411 (3) | C51B—H52B | 0.9600 |
C5A—C51A | 1.492 (3) | C51B—H53B | 0.9600 |
C51A—H51A | 0.9600 | C6B—C7B | 1.363 (3) |
C51A—H52A | 0.9600 | C6B—H6B | 0.9300 |
C51A—H53A | 0.9600 | C7B—N8B | 1.362 (2) |
C6A—C7A | 1.360 (3) | C7B—C71B | 1.479 (3) |
C6A—H6A | 0.9300 | C71B—H71B | 0.9600 |
C7A—N8A | 1.365 (2) | C71B—H72B | 0.9600 |
C7A—C71A | 1.479 (3) | C71B—H73B | 0.9600 |
C71A—H71A | 0.9600 | O1W—H11W | 0.844 (9) |
C71A—H72A | 0.9600 | O1W—H12W | 0.843 (9) |
| | | |
Cl3—Co—Cl4 | 112.31 (3) | C3aA—N8A—N1A | 111.43 (14) |
Cl3—Co—Cl2 | 107.13 (2) | C7A—N8A—N1A | 127.10 (15) |
Cl4—Co—Cl2 | 108.47 (3) | C2B—N1B—N8B | 102.66 (16) |
Cl3—Co—Cl1 | 112.49 (2) | N1B—C2B—N3B | 113.79 (18) |
Cl4—Co—Cl1 | 104.59 (2) | N1B—C2B—H2B | 122.9 |
Cl2—Co—Cl1 | 111.86 (2) | N3B—C2B—H2B | 123.3 |
C2A—N1A—N8A | 102.88 (14) | C3aB—N3B—C2B | 106.35 (17) |
N1A—C2A—N3A | 113.40 (17) | C3aB—N3B—H3B | 126.8 |
N1A—C2A—H2A | 123.2 | C2B—N3B—H3B | 126.8 |
N3A—C2A—H2A | 123.4 | N4B—C3aB—N3B | 128.83 (19) |
C3aA—N3A—C2A | 106.80 (15) | N4B—C3aB—N8B | 125.44 (17) |
C3aA—N3A—H3A | 126.6 | N3B—C3aB—N8B | 105.73 (16) |
C2A—N3A—H3A | 126.6 | C3aB—N4B—C5B | 114.52 (18) |
N4A—C3aA—N3A | 128.99 (16) | N4B—C5B—C6B | 122.37 (18) |
N4A—C3aA—N8A | 125.53 (16) | N4B—C5B—C51B | 116.4 (2) |
N3A—C3aA—N8A | 105.48 (15) | C6B—C5B—C51B | 121.3 (2) |
C3aA—N4A—C5A | 114.64 (16) | C5B—C51B—H51B | 110.0 |
N4A—C5A—C6A | 122.39 (17) | C5B—C51B—H52B | 109.0 |
N4A—C5A—C51A | 117.38 (18) | H51B—C51B—H52B | 109.5 |
C6A—C5A—C51A | 120.23 (18) | C5B—C51B—H53B | 109.4 |
C5A—C51A—H51A | 109.7 | H51B—C51B—H53B | 109.5 |
C5A—C51A—H52A | 109.2 | H52B—C51B—H53B | 109.5 |
H51A—C51A—H52A | 109.5 | C7B—C6B—C5B | 121.60 (19) |
C5A—C51A—H53A | 109.5 | C7B—C6B—H6B | 119.4 |
H51A—C51A—H53A | 109.5 | C5B—C6B—H6B | 119.0 |
H52A—C51A—H53A | 109.5 | N8B—C7B—C6B | 114.45 (18) |
C7A—C6A—C5A | 121.38 (17) | N8B—C7B—C71B | 118.40 (18) |
C7A—C6A—H6A | 119.4 | C6B—C7B—C71B | 127.14 (19) |
C5A—C6A—H6A | 119.2 | C7B—C71B—H71B | 109.6 |
C6A—C7A—N8A | 114.60 (16) | C7B—C71B—H72B | 109.6 |
C6A—C7A—C71A | 126.78 (18) | H71B—C71B—H72B | 109.5 |
N8A—C7A—C71A | 118.62 (18) | C7B—C71B—H73B | 109.3 |
C7A—C71A—H71A | 109.1 | H71B—C71B—H73B | 109.5 |
C7A—C71A—H72A | 109.5 | H72B—C71B—H73B | 109.5 |
H71A—C71A—H72A | 109.5 | C3aB—N8B—C7B | 121.59 (16) |
C7A—C71A—H73A | 109.8 | C3aB—N8B—N1B | 111.47 (15) |
H71A—C71A—H73A | 109.5 | C7B—N8B—N1B | 126.92 (16) |
H72A—C71A—H73A | 109.5 | H11W—O1W—H12W | 108.6 (15) |
C3aA—N8A—C7A | 121.41 (16) | | |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
N3A—H3A···O1Wi | 0.86 | 1.83 | 2.681 (2) | 171 |
N3B—H3B···Cl1 | 0.86 | 2.31 | 3.1325 (18) | 160 |
O1W—H11W···N1Aii | 0.84 (1) | 2.19 (1) | 3.026 (2) | 169 (2) |
O1W—H12W···Cl2 | 0.84 (1) | 2.59 (2) | 3.3122 (15) | 144 (2) |
Symmetry codes: (i) −x, −y+1, −z; (ii) −x+1, −y+1, −z. |