Poly[[bis­(μ₂-3,5-diamino-1,2,4-triazole)-κ²N²:N⁴;κ²N⁴:N²-μ₂-sulfato-κ²O:O′-cadmium(II)] monohydrate]

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 Cd^II atoms, forming infinite strands running in the c-axis direction. The three-dimensional supra­molecular structure is stabilized by N—H...O and O—H...N inter­actions. The two independent water mol­ecules lie on different twofold axes and inter­act with the network through hydrogen bonds.

Key indicators

• Single-crystal X-ray study
• T = 295 K
• Mean [sigma](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

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Computing details

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]

Crystal data

[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) Å^3	Block, colorless
Z = 16	0.47 × 0.19 × 0.14 mm
F(000) = 3360

Data collection

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

Refinement on F^2	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F^2 > 2σ(F^2)] = 0.032	H-atom parameters constrained
wR(F^2) = 0.085	w = 1/[σ^2(Fo^2) + (0.0603P)^2 + 5.4574P] where P = (Fo^2 + 2Fc^2)/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 (Ų)

	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 (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
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)

Cd1—O1	2.354 (7)	N6—C4	1.360 (7)
Cd1—O2^i	2.308 (7)	N7—C3	1.353 (7)
Cd1—N1	2.377 (4)	N8—C3	1.343 (6)
Cd1—N4^ii	2.341 (4)	N8—N9	1.395 (6)
Cd1—N6	2.344 (4)	N9—C4	1.320 (7)
Cd1—N9^iii	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—O2^i	171.3 (2)	C3—N8—N9	109.1 (4)
O1—Cd1—N1	84.1 (2)	C4—N9—N8	102.6 (4)
O1—Cd1—N4^ii	85.2 (2)	C4—N9—Cd1^vi	138.2 (4)
O1—Cd1—N6	81.6 (2)	N8—N9—Cd1^vi	117.3 (3)
O1—Cd1—N9^iii	90.3 (2)	N2—C1—N1	126.7 (4)
O2^i—Cd1—N1	88.4 (2)	N2—C1—N3	123.3 (4)
O2^i—Cd1—N4^ii	102.6 (2)	N1—C1—N3	109.9 (4)
O2^i—Cd1—N6	94.3 (2)	N4—C2—N1	114.7 (5)
O2^i—Cd1—N9^iii	93.5 (2)	N4—C2—N5	123.9 (5)
N1—Cd1—N4^ii	168.1 (2)	N1—C2—N5	121.4 (5)
N1—Cd1—N6	90.9 (1)	N8—C3—N6	109.9 (4)
N1—Cd1—N9^iii	86.1 (1)	N8—C3—N7	122.8 (5)
N4^ii—Cd1—N6	92.8 (1)	N6—C3—N7	127.3 (4)
N4^ii—Cd1—N9^iii	88.7 (1)	N9—C4—N6	114.8 (5)
N6—Cd1—N9^iii	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—Cd1^iv	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—Cd1^v	137.5 (4)	N9—N8—H8	125.5
N3—N4—Cd1^v	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—Cd1^vi	164.1 (3)
O4—S1—O1—Cd1	−60.5 (5)	C2—N1—C1—N2	−177.7 (5)
N4^ii—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)
N9^iii—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—Cd1^iv	174.4 (4)	N4—N3—C1—N1	0.5 (6)
O3—S1—O2—Cd1^iv	−67.3 (6)	N3—N4—C2—N1	0.1 (6)
O4—S1—O2—Cd1^iv	55.7 (6)	Cd1^v—N4—C2—N1	−158.4 (4)
O2^i—Cd1—N1—C1	−148.4 (4)	N3—N4—C2—N5	179.6 (5)
N4^ii—Cd1—N1—C1	53.9 (9)	Cd1^v—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)
N9^iii—Cd1—N1—C1	118.1 (4)	C1—N1—C2—N5	−179.3 (5)
O2^i—Cd1—N1—C2	43.1 (4)	Cd1—N1—C2—N5	−8.5 (7)
N4^ii—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)
N9^iii—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—Cd1^v	163.5 (3)	Cd1—N6—C3—N7	13.0 (7)
O2^i—Cd1—N6—C3	−161.2 (4)	N8—N9—C4—N6	1.4 (6)
N4^ii—Cd1—N6—C3	−58.3 (4)	Cd1^vi—N9—C4—N6	−161.2 (4)
O1—Cd1—N6—C3	26.4 (4)	N8—N9—C4—N10	−178.8 (5)
N9^iii—Cd1—N6—C3	41.7 (12)	Cd1^vi—N9—C4—N10	18.6 (9)
N1—Cd1—N6—C3	110.3 (4)	C3—N6—C4—N9	0.6 (6)
O2^i—Cd1—N6—C4	36.0 (5)	Cd1—N6—C4—N9	166.6 (3)
N4^ii—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)

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···O3^v	0.85	2.07	2.837 (6)	150
N5—H5a···O3^vii	0.85	2.05	2.857 (6)	157
N5—H5b···O2^i	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···O4^vi	0.85	2.13	2.783 (6)	133
N10—H10a···O4^viii	0.85	2.02	2.826 (6)	159
N10—H10b···O2^i	0.85	2.32	3.106 (9)	154
O1w—H1w···N5^iv	0.85	2.31	3.000 (5)	138
O2w—H2w···N10^iv	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.