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metal-organic compounds
The geometry of the Cd atom in the polymeric title complex, {[Cd(SO4)(C2H5N5)2]·H2O}n, is six-coordinate distorted octahedral, defined by two O-atom donors derived from two sulfate dianions and four N atoms from four different 3,5-diamino-1,2,4-triazole ligands. The sulfate dianions interact with CdII atoms, forming infinite strands running in the c-axis direction. The three-dimensional supramolecular structure is stabilized by N—HO and O—HN interactions. The two independent water molecules lie on different twofold axes and interact with the network through hydrogen bonds.
Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806029096/tk2060sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536806029096/tk2060Isup2.hkl |
CCDC reference: 621508
Key indicators
- Single-crystal X-ray study
- T = 295 K
- Mean (N-C) = 0.007 Å
- R factor = 0.032
- wR factor = 0.085
- Data-to-parameter ratio = 11.1
checkCIF/PLATON results
No syntax errors found
Alert level B PLAT417_ALERT_2_B Short Inter D-H..H-D H7A .. H7A .. 2.06 Ang. PLAT417_ALERT_2_B Short Inter D-H..H-D H1W .. H5A .. 1.94 Ang. PLAT417_ALERT_2_B Short Inter D-H..H-D H2W .. H10A .. 1.96 Ang.
Alert level C PLAT062_ALERT_4_C Rescale T(min) & T(max) by ..................... 0.99 PLAT152_ALERT_1_C Supplied and Calc Volume s.u. Inconsistent ..... ? PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 26 N9 -CD1 -N6 -C3 41.70 1.20 13.554 1.555 1.555 1.555
Alert level G REFLT03_ALERT_4_G Please check that the estimate of the number of Friedel pairs is correct. If it is not, please give the correct count in the _publ_section_exptl_refinement section of the submitted CIF. From the CIF: _diffrn_reflns_theta_max 25.00 From the CIF: _reflns_number_total 2121 Count of symmetry unique reflns 1135 Completeness (_total/calc) 186.87% TEST3: Check Friedels for noncentro structure Estimate of Friedel pairs measured 986 Fraction of Friedel pairs measured 0.869 Are heavy atom types Z>Si present yes
0 ALERT level A = In general: serious problem 3 ALERT level B = Potentially serious problem 3 ALERT level C = Check and explain 1 ALERT level G = General alerts; check 1 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 3 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check
Computing details top
Data collection: SMART (Bruker, 2004); cell refinement: SAINT (Bruker, 2004); 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.
Poly[[bis(µ2-3,5-diamino-1,2,4-triazole)-
κ2N2:N4;κ2N4:N2–
µ2-sulfato-κ2O:O'-cadmium(II)] monohydrate] top
Crystal data top
[Cd(SO4)(C2H5N5)2]·H2O | Dx = 2.231 Mg m−3 |
Mr = 424.70 | Mo Kα radiation, λ = 0.71073 Å |
Tetragonal, I41cd | Cell parameters from 4515 reflections |
Hall symbol: I 4bw -2c | θ = 2.9–26.9° |
a = 13.446 (1) Å | µ = 1.94 mm−1 |
c = 27.980 (2) Å | T = 295 K |
V = 5058.5 (5) Å3 | Block, colorless |
Z = 16 | 0.47 × 0.19 × 0.14 mm |
F(000) = 3360 |
Data collection top
Bruker APEX-II area-detector diffractometer | 2121 independent reflections |
Radiation source: fine-focus sealed tube | 1966 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.029 |
φ and ω scans | θmax = 25.0°, θmin = 2.6° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −14→15 |
Tmin = 0.463, Tmax = 0.773 | k = −15→15 |
11734 measured reflections | l = −33→28 |
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)] = 0.032 | H-atom parameters constrained |
wR(F2) = 0.085 | w = 1/[σ2(Fo2) + (0.0603P)2 + 5.4574P] where P = (Fo2 + 2Fc2)/3 |
S = 1.08 | (Δ/σ)max = 0.001 |
2121 reflections | Δρmax = 2.06 e Å−3 |
191 parameters | Δρmin = −1.10 e Å−3 |
1 restraint | Absolute structure: Flack (1983), 986 Friedel pairs |
Primary atom site location: structure-invariant direct methods | Absolute structure parameter: 0.04 (3) |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
x | y | z | Uiso*/Ueq | ||
Cd1 | 0.24126 (5) | 0.23814 (4) | 0.50001 (4) | 0.0179 (2) | |
S1 | 0.2464 (1) | 0.2930 (1) | 0.6271 (1) | 0.0276 (3) | |
O1 | 0.2333 (4) | 0.2326 (4) | 0.5840 (3) | 0.028 (1) | |
O2 | 0.2256 (5) | 0.2324 (4) | 0.6687 (3) | 0.039 (1) | |
O3 | 0.1752 (3) | 0.3759 (3) | 0.6254 (2) | 0.054 (1) | |
O4 | 0.3505 (3) | 0.3288 (4) | 0.6282 (2) | 0.051 (1) | |
O1w | 0.5000 | 0.0000 | 0.6683 (4) | 0.051 (3) | |
O2w | 0.0000 | 0.0000 | 0.6695 (4) | 0.059 (3) | |
N1 | 0.4108 (3) | 0.1944 (3) | 0.5118 (2) | 0.023 (1) | |
N2 | 0.4059 (3) | 0.0937 (3) | 0.5812 (2) | 0.037 (1) | |
N3 | 0.5514 (3) | 0.1483 (3) | 0.5441 (2) | 0.028 (1) | |
N4 | 0.5772 (3) | 0.2043 (3) | 0.5043 (2) | 0.024 (1) | |
N5 | 0.4773 (3) | 0.2861 (4) | 0.4468 (2) | 0.034 (1) | |
N6 | 0.1928 (3) | 0.0716 (3) | 0.5087 (2) | 0.023 (1) | |
N7 | 0.0918 (4) | 0.0797 (3) | 0.5799 (2) | 0.042 (1) | |
N8 | 0.1442 (3) | −0.0685 (3) | 0.5419 (2) | 0.029 (1) | |
H8 | 0.1141 | −0.1086 | 0.5603 | 0.035* | |
N9 | 0.2042 (3) | −0.0955 (3) | 0.5033 (2) | 0.027 (1) | |
N10 | 0.2876 (4) | 0.0022 (4) | 0.4452 (2) | 0.036 (1) | |
C1 | 0.4524 (3) | 0.1442 (3) | 0.5477 (2) | 0.024 (1) | |
C2 | 0.4898 (4) | 0.2293 (4) | 0.4867 (2) | 0.022 (1) | |
C3 | 0.1417 (3) | 0.0312 (3) | 0.5450 (2) | 0.023 (1) | |
C4 | 0.2294 (4) | −0.0087 (4) | 0.4849 (2) | 0.024 (1) | |
H1w | 0.4517 | −0.0181 | 0.6856 | 0.062* | |
H2w | −0.0061 | 0.0514 | 0.6868 | 0.071* | |
H2a | 0.3427 | 0.0909 | 0.5812 | 0.044* | |
H2b | 0.4389 | 0.0640 | 0.6028 | 0.044* | |
H3 | 0.5922 | 0.1209 | 0.5632 | 0.033* | |
H5a | 0.5278 | 0.3077 | 0.4317 | 0.040* | |
H5b | 0.4191 | 0.3001 | 0.4371 | 0.040* | |
H7a | 0.0603 | 0.0470 | 0.6011 | 0.051* | |
H7b | 0.0919 | 0.1429 | 0.5807 | 0.051* | |
H10a | 0.3099 | −0.0489 | 0.4308 | 0.043* | |
H10b | 0.3015 | 0.0600 | 0.4349 | 0.043* |
Atomic displacement parameters (Å2) top
U11 | U22 | U33 | U12 | U13 | U23 | |
Cd1 | 0.0189 (3) | 0.0181 (3) | 0.0165 (2) | −0.0009 (1) | 0.0012 (4) | −0.0009 (5) |
S1 | 0.0327 (8) | 0.0276 (8) | 0.0223 (8) | −0.0017 (6) | −0.0045 (5) | −0.0004 (6) |
O1 | 0.035 (3) | 0.031 (3) | 0.018 (3) | 0.002 (2) | 0.002 (2) | −0.001 (2) |
O2 | 0.058 (3) | 0.038 (3) | 0.019 (3) | −0.010 (3) | 0.002 (2) | −0.006 (2) |
O3 | 0.059 (3) | 0.048 (3) | 0.054 (3) | 0.024 (2) | −0.030 (2) | −0.023 (2) |
O4 | 0.045 (2) | 0.067 (3) | 0.041 (3) | −0.019 (2) | −0.021 (2) | 0.022 (2) |
O1w | 0.029 (3) | 0.088 (5) | 0.037 (6) | −0.005 (3) | 0.000 | 0.000 |
O2w | 0.097 (6) | 0.037 (3) | 0.043 (6) | 0.009 (3) | 0.000 | 0.000 |
N1 | 0.018 (2) | 0.026 (2) | 0.025 (2) | 0.000 (2) | 0.001 (2) | 0.000 (2) |
N2 | 0.026 (2) | 0.041 (3) | 0.043 (3) | 0.004 (2) | 0.007 (2) | 0.017 (2) |
N3 | 0.020 (2) | 0.028 (2) | 0.035 (2) | 0.001 (2) | −0.004 (2) | 0.012 (2) |
N4 | 0.020 (2) | 0.026 (2) | 0.026 (2) | −0.003 (2) | 0.000 (2) | 0.007 (2) |
N5 | 0.024 (3) | 0.050 (3) | 0.027 (3) | 0.007 (2) | 0.003 (2) | 0.020 (2) |
N6 | 0.026 (2) | 0.016 (2) | 0.025 (2) | −0.002 (2) | 0.003 (2) | −0.004 (2) |
N7 | 0.049 (3) | 0.031 (2) | 0.047 (3) | −0.010 (2) | 0.015 (3) | −0.014 (2) |
N8 | 0.031 (2) | 0.023 (2) | 0.033 (2) | 0.001 (2) | 0.007 (2) | 0.006 (2) |
N9 | 0.025 (2) | 0.020 (2) | 0.035 (3) | 0.004 (2) | 0.006 (2) | 0.002 (2) |
N10 | 0.048 (3) | 0.028 (2) | 0.032 (3) | −0.002 (2) | 0.020 (2) | −0.002 (2) |
C1 | 0.025 (3) | 0.021 (2) | 0.026 (3) | 0.006 (2) | −0.002 (2) | 0.004 (2) |
C2 | 0.028 (3) | 0.019 (2) | 0.019 (3) | 0.001 (2) | 0.002 (2) | 0.002 (2) |
C3 | 0.019 (2) | 0.026 (2) | 0.023 (3) | 0.000 (2) | 0.003 (2) | 0.005 (2) |
C4 | 0.023 (2) | 0.030 (3) | 0.018 (3) | 0.000 (2) | 0.004 (2) | −0.001 (2) |
Geometric parameters (Å, º) top
Cd1—O1 | 2.354 (7) | N6—C4 | 1.360 (7) |
Cd1—O2i | 2.308 (7) | N7—C3 | 1.353 (7) |
Cd1—N1 | 2.377 (4) | N8—C3 | 1.343 (6) |
Cd1—N4ii | 2.341 (4) | N8—N9 | 1.395 (6) |
Cd1—N6 | 2.344 (4) | N9—C4 | 1.320 (7) |
Cd1—N9iii | 2.355 (4) | N10—C4 | 1.367 (7) |
S1—O1 | 1.463 (7) | O1w—H1w | 0.85 |
S1—O2 | 1.449 (7) | O2w—H2w | 0.85 |
S1—O3 | 1.471 (4) | N2—H2a | 0.85 |
S1—O4 | 1.481 (4) | N2—H2b | 0.85 |
N1—C1 | 1.334 (6) | N3—H3 | 0.85 |
N1—C2 | 1.357 (7) | N5—H5a | 0.85 |
N2—C1 | 1.315 (7) | N5—H5b | 0.85 |
N3—C1 | 1.335 (6) | N7—H7a | 0.85 |
N3—N4 | 1.390 (6) | N7—H7b | 0.85 |
N4—C2 | 1.317 (7) | N8—H8 | 0.85 |
N5—C2 | 1.363 (7) | N10—H10a | 0.85 |
N6—C3 | 1.343 (6) | N10—H10b | 0.85 |
O1—Cd1—O2i | 171.3 (2) | C3—N8—N9 | 109.1 (4) |
O1—Cd1—N1 | 84.1 (2) | C4—N9—N8 | 102.6 (4) |
O1—Cd1—N4ii | 85.2 (2) | C4—N9—Cd1vi | 138.2 (4) |
O1—Cd1—N6 | 81.6 (2) | N8—N9—Cd1vi | 117.3 (3) |
O1—Cd1—N9iii | 90.3 (2) | N2—C1—N1 | 126.7 (4) |
O2i—Cd1—N1 | 88.4 (2) | N2—C1—N3 | 123.3 (4) |
O2i—Cd1—N4ii | 102.6 (2) | N1—C1—N3 | 109.9 (4) |
O2i—Cd1—N6 | 94.3 (2) | N4—C2—N1 | 114.7 (5) |
O2i—Cd1—N9iii | 93.5 (2) | N4—C2—N5 | 123.9 (5) |
N1—Cd1—N4ii | 168.1 (2) | N1—C2—N5 | 121.4 (5) |
N1—Cd1—N6 | 90.9 (1) | N8—C3—N6 | 109.9 (4) |
N1—Cd1—N9iii | 86.1 (1) | N8—C3—N7 | 122.8 (5) |
N4ii—Cd1—N6 | 92.8 (1) | N6—C3—N7 | 127.3 (4) |
N4ii—Cd1—N9iii | 88.7 (1) | N9—C4—N6 | 114.8 (5) |
N6—Cd1—N9iii | 171.6 (2) | N9—C4—N10 | 123.9 (5) |
O2—S1—O1 | 109.1 (3) | N6—C4—N10 | 121.3 (5) |
O2—S1—O3 | 109.1 (3) | C1—N2—H2a | 120.0 |
O1—S1—O3 | 108.4 (3) | C1—N2—H2b | 120.0 |
O2—S1—O4 | 110.4 (3) | H2a—N2—H2b | 120.0 |
O1—S1—O4 | 108.1 (3) | C1—N3—H3 | 125.3 |
O3—S1—O4 | 111.6 (2) | N4—N3—H3 | 125.3 |
S1—O1—Cd1 | 143.0 (4) | C2—N5—H5a | 120.0 |
S1—O2—Cd1iv | 133.8 (4) | C2—N5—H5b | 120.0 |
C1—N1—C2 | 103.6 (4) | H5a—N5—H5b | 120.0 |
C1—N1—Cd1 | 129.2 (3) | C3—N7—H7a | 120.0 |
C2—N1—Cd1 | 126.4 (3) | C3—N7—H7b | 120.0 |
C1—N3—N4 | 109.4 (4) | H7a—N7—H7b | 120.0 |
C2—N4—N3 | 102.4 (4) | C3—N8—H8 | 125.5 |
C2—N4—Cd1v | 137.5 (4) | N9—N8—H8 | 125.5 |
N3—N4—Cd1v | 117.1 (3) | C4—N10—H10a | 120.0 |
C3—N6—C4 | 103.5 (4) | C4—N10—H10b | 120.0 |
C3—N6—Cd1 | 127.4 (3) | H10a—N10—H10b | 120.0 |
C4—N6—Cd1 | 127.4 (3) | ||
O2—S1—O1—Cd1 | 179.4 (5) | C3—N8—N9—C4 | −2.9 (5) |
O3—S1—O1—Cd1 | 60.7 (5) | C3—N8—N9—Cd1vi | 164.1 (3) |
O4—S1—O1—Cd1 | −60.5 (5) | C2—N1—C1—N2 | −177.7 (5) |
N4ii—Cd1—O1—S1 | −85.7 (5) | Cd1—N1—C1—N2 | 11.8 (7) |
N6—Cd1—O1—S1 | −179.2 (5) | C2—N1—C1—N3 | −0.4 (5) |
N9iii—Cd1—O1—S1 | 3.0 (5) | Cd1—N1—C1—N3 | −171.0 (3) |
N1—Cd1—O1—S1 | 89.0 (5) | N4—N3—C1—N2 | 177.8 (5) |
O1—S1—O2—Cd1iv | 174.4 (4) | N4—N3—C1—N1 | 0.5 (6) |
O3—S1—O2—Cd1iv | −67.3 (6) | N3—N4—C2—N1 | 0.1 (6) |
O4—S1—O2—Cd1iv | 55.7 (6) | Cd1v—N4—C2—N1 | −158.4 (4) |
O2i—Cd1—N1—C1 | −148.4 (4) | N3—N4—C2—N5 | 179.6 (5) |
N4ii—Cd1—N1—C1 | 53.9 (9) | Cd1v—N4—C2—N5 | 21.2 (9) |
N6—Cd1—N1—C1 | −54.1 (4) | C1—N1—C2—N4 | 0.2 (6) |
O1—Cd1—N1—C1 | 27.3 (4) | Cd1—N1—C2—N4 | 171.1 (3) |
N9iii—Cd1—N1—C1 | 118.1 (4) | C1—N1—C2—N5 | −179.3 (5) |
O2i—Cd1—N1—C2 | 43.1 (4) | Cd1—N1—C2—N5 | −8.5 (7) |
N4ii—Cd1—N1—C2 | −114.7 (7) | N9—N8—C3—N6 | 3.5 (6) |
N6—Cd1—N1—C2 | 137.3 (4) | N9—N8—C3—N7 | −177.9 (5) |
O1—Cd1—N1—C2 | −141.2 (4) | C4—N6—C3—N8 | −2.5 (5) |
N9iii—Cd1—N1—C2 | −50.5 (4) | Cd1—N6—C3—N8 | −168.4 (3) |
C1—N3—N4—C2 | −0.3 (5) | C4—N6—C3—N7 | 179.0 (5) |
C1—N3—N4—Cd1v | 163.5 (3) | Cd1—N6—C3—N7 | 13.0 (7) |
O2i—Cd1—N6—C3 | −161.2 (4) | N8—N9—C4—N6 | 1.4 (6) |
N4ii—Cd1—N6—C3 | −58.3 (4) | Cd1vi—N9—C4—N6 | −161.2 (4) |
O1—Cd1—N6—C3 | 26.4 (4) | N8—N9—C4—N10 | −178.8 (5) |
N9iii—Cd1—N6—C3 | 41.7 (12) | Cd1vi—N9—C4—N10 | 18.6 (9) |
N1—Cd1—N6—C3 | 110.3 (4) | C3—N6—C4—N9 | 0.6 (6) |
O2i—Cd1—N6—C4 | 36.0 (5) | Cd1—N6—C4—N9 | 166.6 (3) |
N4ii—Cd1—N6—C4 | 138.9 (4) | C3—N6—C4—N10 | −179.2 (5) |
O1—Cd1—N6—C4 | −136.3 (5) | Cd1—N6—C4—N10 | −13.3 (8) |
N1—Cd1—N6—C4 | −52.4 (5) |
Symmetry codes: (i) −y+1/2, x, z−1/4; (ii) x−1/2, −y+1/2, z; (iii) −x+1/2, y+1/2, z; (iv) y, −x+1/2, z+1/4; (v) x+1/2, −y+1/2, z; (vi) −x+1/2, y−1/2, z. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
N2—H2a···O1 | 0.85 | 2.41 | 2.979 (6) | 125 |
N2—H2b···O1w | 0.85 | 2.18 | 3.02 (1) | 168 |
N3—H3···O3v | 0.85 | 2.07 | 2.837 (6) | 150 |
N5—H5a···O3vii | 0.85 | 2.05 | 2.857 (6) | 157 |
N5—H5b···O2i | 0.85 | 2.33 | 3.039 (7) | 142 |
N7—H7a···O2w | 0.85 | 2.17 | 2.99 (1) | 162 |
N7—H7b···O1 | 0.85 | 2.25 | 2.803 (8) | 123 |
N8—H8···O4vi | 0.85 | 2.13 | 2.783 (6) | 133 |
N10—H10a···O4viii | 0.85 | 2.02 | 2.826 (6) | 159 |
N10—H10b···O2i | 0.85 | 2.32 | 3.106 (9) | 154 |
O1w—H1w···N5iv | 0.85 | 2.31 | 3.000 (5) | 138 |
O2w—H2w···N10iv | 0.85 | 2.18 | 2.946 (6) | 150 |
Symmetry codes: (i) −y+1/2, x, z−1/4; (iv) y, −x+1/2, z+1/4; (v) x+1/2, −y+1/2, z; (vi) −x+1/2, y−1/2, z; (vii) −y+1, −x+1/2, z−1/4; (viii) y, x−1/2, z−1/4. |
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