A new cadmium coordination polymer based on 4-amino-4H-1,2,4-triazole

Said, M.; Boughzala, H.

doi:10.1107/S2056989018000464

A new cadmium coordination polymer based on 4-amino-4H-1,2,4-triazole

Here we report the chemical synthesis and crystal structure of a new hybrid chloro-cadmium coordination polymer based on 4-amino-4H-1,2,4 triazole solved by single-crystal X-ray diffraction. With an unusual architecture, the crystal structure exhibits two distorted octahedral coordinations of Cd^II joined by edge sharing. The first is composed by four chlorine and two N atoms from the triazole ligands. The second is formed by five Cl atoms and by one N atom from the triazole ligand.

Keywords: crystal structure; hybrid coordination polymer; cadmium(II); triazole.

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Supporting information

	Crystallographic Information File (CIF) https://doi.org/10.1107/S2056989018000464/xi2006sup1.cif Contains datablock I
	Structure factor file (CIF format) https://doi.org/10.1107/S2056989018000464/xi2006Isup2.hkl Contains datablock I

CCDC reference: 1810807

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Key indicators

Single-crystal X-ray study
T = 298 K
Mean (N-N) = 0.009 Å
R factor = 0.040
wR factor = 0.123
Data-to-parameter ratio = 16.5

checkCIF/PLATON results

No syntax errors found



Alert level C
PLAT352_ALERT_3_C Short  N-H (X0.87,N1.01A)  N5       - H5       .       0.75 Ang.
PLAT353_ALERT_3_C Long   N-H (N0.87,N1.01A)  N4       - H4A      .       1.04 Ang.
PLAT972_ALERT_2_C Check Calcd Resid. Dens.  0.81A   From Cd1            -1.85 eA-3
PLAT972_ALERT_2_C Check Calcd Resid. Dens.  0.82A   From Cd1            -1.70 eA-3
PLAT972_ALERT_2_C Check Calcd Resid. Dens.  0.92A   From Cd2            -1.57 eA-3
PLAT978_ALERT_2_C Number C-C Bonds with Positive Residual Density.          0 Info

Alert level G
PLAT002_ALERT_2_G Number of Distance or Angle Restraints on AtSite          6 Note
PLAT004_ALERT_5_G Polymeric Structure Found with Maximum Dimension          2 Info
PLAT007_ALERT_5_G Number of Unrefined Donor-H Atoms ..............          3 Report
PLAT042_ALERT_1_G Calc. and Reported MoietyFormula Strings  Differ     Please Check
PLAT063_ALERT_4_G Crystal Size Likely too Large for Beam Size ....       0.71 mm
PLAT164_ALERT_4_G Nr. of Refined C-H H-Atoms in Heavy-Atom Struct.          1 Note
PLAT172_ALERT_4_G The CIF-Embedded .res File Contains DFIX Records          2 Report
PLAT173_ALERT_4_G The CIF-Embedded .res File Contains DANG Records          1 Report
PLAT232_ALERT_2_G Hirshfeld Test Diff (M-X) Cd1      --Cl2_c     .        7.1 s.u.
PLAT720_ALERT_4_G Number of Unusual/Non-Standard Labels ..........          2 Note
PLAT860_ALERT_3_G Number of Least-Squares Restraints .............          5 Note
PLAT910_ALERT_3_G Missing # of FCF Reflection(s) Below Theta(Min).          1 Note
PLAT912_ALERT_4_G Missing # of FCF Reflections Above STh/L=  0.600          2 Note

   0 ALERT level A = Most likely a serious problem - resolve or explain
   0 ALERT level B = A potentially serious problem, consider carefully
   6 ALERT level C = Check. Ensure it is not caused by an omission or oversight
  13 ALERT level G = General information/check it is not something unexpected

   1 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
   6 ALERT type 2 Indicator that the structure model may be wrong or deficient
   4 ALERT type 3 Indicator that the structure quality may be low
   6 ALERT type 4 Improvement, methodology, query or suggestion
   2 ALERT type 5 Informative message, check

Computing details top

Data collection: CAD-4 EXPRESS (Enraf–Nonius, 1994); cell refinement: CAD-4 EXPRESS (Enraf–Nonius, 1994); data reduction: XCAD4 (Harms & Wocadlo, 1995); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL2014 (Sheldrick, 2015); molecular graphics: DIAMOND (Brandenburg, 2006); software used to prepare material for publication: publCIF (Westrip, 2010).

Poly[bis(4-amino-4H-1,2,4-triazolium) [bis(µ₂-4-amino-4H-1,2,4-triazole-κ²N¹:N²)tetra-µ₂-chlorido-tetrachloridotricadmium(II)] dihydrate] top

Crystal data top

(C₂H₅N₄)₂[Cd₃Cl₈(C₂H₄N₄)₂]·2H₂O	F(000) = 956
M_r = 995.21	D_x = 2.298 Mg m⁻³
Monoclinic, P2₁/c	Mo Kα radiation, λ = 0.71073 Å
a = 12.685 (3) Å	Cell parameters from 25 reflections
b = 15.498 (3) Å	θ = 10–15°
c = 7.375 (2) Å	µ = 2.98 mm⁻¹
β = 97.12 (3)°	T = 298 K
V = 1438.6 (6) Å³	Prism, colourless
Z = 2	0.71 × 0.21 × 0.21 mm

Data collection top

Enraf–Nonius CAD-4 diffractometer	R_int = 0.032
Radiation source: Enraf Nonius FR590	θ_max = 27.0°, θ_min = 2.1°
non–profiled ω/2τ scans	h = −16→16
Absorption correction: ψ scan (North et al., 1968)	k = −19→1
T_min = 0.799, T_max = 1.000	l = −9→1
3670 measured reflections	2 standard reflections every 120 min
3136 independent reflections	intensity decay: 8%
2654 reflections with I > 2σ(I)

Refinement top

Refinement on F²	Hydrogen site location: mixed
Least-squares matrix: full	H atoms treated by a mixture of independent and constrained refinement
R[F² > 2σ(F²)] = 0.040	w = 1/[σ²(F_o²) + (0.0848P)² + 1.0345P] where P = (F_o² + 2F_c²)/3
wR(F²) = 0.123	(Δ/σ)_max = 0.001
S = 1.06	Δρ_max = 1.58 e Å⁻³
3136 reflections	Δρ_min = −1.99 e Å⁻³
190 parameters	Extinction correction: SHELXL2014 (Sheldrick, 2015), Fc^*=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4
5 restraints	Extinction coefficient: 0.0041 (7)

Special details top

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds 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 > 2sigma(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	U_iso*/U_eq
Cd1	0.72922 (3)	0.36225 (2)	0.60671 (4)	0.02384 (16)
Cd2	0.5000	0.5000	0.5000	0.02726 (18)
Cl1	0.65520 (10)	0.45547 (8)	0.31268 (16)	0.0291 (3)
Cl2	0.78296 (10)	0.26723 (9)	0.89644 (16)	0.0307 (3)
Cl3	0.63396 (12)	0.47886 (9)	0.79095 (17)	0.0379 (3)
Cl4	0.91217 (11)	0.42626 (9)	0.6250 (2)	0.0369 (3)
N1	0.5591 (3)	0.2978 (3)	0.5599 (6)	0.0271 (9)
N2	0.4709 (4)	0.3474 (3)	0.5015 (6)	0.0300 (9)
N3	0.4303 (4)	0.2130 (3)	0.4573 (6)	0.0284 (9)
N4	0.3704 (5)	0.1390 (3)	0.3952 (8)	0.0427 (12)
N5	1.0964 (5)	0.2603 (4)	0.1439 (8)	0.0406 (11)
N6	1.1503 (5)	0.3284 (4)	0.0808 (9)	0.0552 (15)
N7	0.9940 (4)	0.3688 (3)	0.1463 (6)	0.0341 (10)
N8	0.9074 (4)	0.4233 (3)	0.1599 (6)	0.0388 (11)
C1	0.5314 (4)	0.2172 (3)	0.5326 (7)	0.0301 (10)
H1	0.5755	0.1699	0.5613	0.036*
C2	0.3953 (4)	0.2949 (4)	0.4392 (8)	0.0326 (11)
H2	0.3273	0.3114	0.3895	0.039*
C3	1.0035 (5)	0.2844 (4)	0.1816 (8)	0.0371 (12)
H3	0.9528	0.2493	0.2253	0.044*
C4	1.0865 (6)	0.3931 (4)	0.0848 (11)	0.0481 (16)
O1W	0.1792 (5)	0.3900 (4)	0.5653 (10)	0.0663 (15)
H4	1.103 (5)	0.450 (4)	0.066 (9)	0.038 (17)*
H5	1.127 (6)	0.219 (5)	0.158 (11)	0.05 (2)*
H8A	0.8524	0.4002	0.1015	0.050*
H8B	0.9153	0.4271	0.2827	0.050*
H4A	0.4298	0.0977	0.3612	0.050*
H4B	0.350 (6)	0.120 (4)	0.516 (11)	0.045 (19)*
HW2	0.237 (4)	0.396 (5)	0.638 (9)	0.07 (3)*
HW1	0.142 (6)	0.435 (4)	0.580 (14)	0.11 (4)*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Cd1	0.0255 (2)	0.0249 (2)	0.0204 (2)	0.00043 (12)	0.00023 (14)	0.00166 (12)
Cd2	0.0335 (3)	0.0216 (3)	0.0261 (3)	0.00527 (19)	0.0016 (2)	0.00027 (18)
Cl1	0.0363 (6)	0.0285 (6)	0.0229 (5)	0.0036 (5)	0.0046 (5)	0.0044 (4)
Cl2	0.0347 (6)	0.0341 (7)	0.0227 (6)	−0.0022 (5)	0.0013 (5)	0.0100 (5)
Cl3	0.0507 (8)	0.0372 (7)	0.0235 (6)	0.0143 (6)	−0.0041 (5)	−0.0085 (5)
Cl4	0.0327 (7)	0.0366 (7)	0.0410 (7)	−0.0101 (5)	0.0027 (5)	−0.0007 (6)
N1	0.026 (2)	0.026 (2)	0.029 (2)	0.0019 (16)	0.0020 (16)	0.0019 (16)
N2	0.032 (2)	0.029 (2)	0.028 (2)	0.0029 (18)	0.0022 (17)	−0.0003 (17)
N3	0.040 (2)	0.025 (2)	0.022 (2)	−0.0059 (18)	0.0095 (17)	−0.0032 (15)
N4	0.054 (3)	0.034 (3)	0.042 (3)	−0.020 (2)	0.011 (2)	−0.009 (2)
N5	0.046 (3)	0.034 (3)	0.041 (3)	−0.001 (2)	0.003 (2)	0.000 (2)
N6	0.054 (3)	0.047 (3)	0.071 (4)	0.002 (3)	0.031 (3)	0.005 (3)
N7	0.035 (2)	0.043 (3)	0.025 (2)	−0.0025 (19)	0.0072 (18)	−0.0042 (18)
N8	0.044 (3)	0.034 (2)	0.040 (3)	−0.002 (2)	0.009 (2)	−0.006 (2)
C1	0.034 (3)	0.025 (2)	0.031 (3)	0.003 (2)	0.002 (2)	0.002 (2)
C2	0.030 (3)	0.034 (3)	0.034 (3)	−0.001 (2)	0.003 (2)	−0.001 (2)
C3	0.042 (3)	0.037 (3)	0.031 (3)	−0.007 (2)	0.001 (2)	0.007 (2)
C4	0.051 (4)	0.037 (3)	0.061 (4)	−0.007 (3)	0.023 (3)	0.000 (3)
O1W	0.057 (3)	0.043 (3)	0.095 (5)	−0.011 (3)	−0.002 (3)	−0.002 (3)

Geometric parameters (Å, º) top

Cd1—N1	2.365 (4)	N4—H4A	1.0400
Cd1—Cl4	2.5120 (14)	N4—H4B	1.01 (8)
Cd1—Cl2	2.6148 (13)	N5—C3	1.299 (9)
Cd1—Cl3	2.6418 (14)	N5—N6	1.369 (8)
Cd1—Cl2ⁱ	2.6754 (13)	N5—H5	0.75 (8)
Cd1—Cl1	2.6769 (14)	N6—C4	1.292 (9)
Cd2—N2ⁱⁱ	2.393 (5)	N7—C3	1.336 (7)
Cd2—N2	2.393 (5)	N7—C4	1.362 (8)
Cd2—Cl3	2.5874 (16)	N7—N8	1.399 (7)
Cd2—Cl3ⁱⁱ	2.5875 (16)	N8—H8A	0.850
Cd2—Cl1	2.6332 (14)	N8—H8B	0.900
Cd2—Cl1ⁱⁱ	2.6333 (14)	C1—H1	0.9300
N1—C1	1.306 (7)	C2—H2	0.9300
N1—N2	1.382 (6)	C3—H3	0.9300
N2—C2	1.297 (7)	C4—H4	0.92 (6)
N3—C1	1.335 (7)	O1W—HW2	0.862 (10)
N3—C2	1.346 (7)	O1W—HW1	0.857 (10)
N3—N4	1.419 (6)

N1—Cd1—Cl4	174.37 (11)	N1—N2—Cd2	115.6 (3)
Cl4—Cd1—Cl3	100.40 (5)	C1—N3—C2	106.4 (4)
Cl2—Cd1—Cl3	93.13 (5)	C1—N3—N4	128.4 (5)
N1—Cd1—Cl2ⁱ	83.80 (11)	C2—N3—N4	125.0 (5)
Cl4—Cd1—Cl2ⁱ	91.57 (5)	N3—N4—H4A	102.00
Cl2—Cd1—Cl2ⁱ	89.53 (3)	N3—N4—H4B	98 (4)
N1—Cd1—Cl1	83.54 (11)	H4A—N4—H4B	108.00
Cl4—Cd1—Cl1	93.40 (5)	C3—N5—N6	110.8 (5)
Cl2—Cd1—Cl1	174.60 (4)	C3—N5—H5	133 (6)
Cl3—Cd1—Cl1	84.86 (4)	N6—N5—H5	116 (6)
Cl2ⁱ—Cd1—Cl1	91.39 (4)	C4—N6—N5	104.5 (6)
N2ⁱⁱ—Cd2—Cl3	92.46 (11)	C3—N7—C4	106.0 (5)
N2—Cd2—Cl3	87.54 (12)	C3—N7—N8	129.0 (5)
N2ⁱⁱ—Cd2—Cl3ⁱⁱ	87.54 (11)	C4—N7—N8	125.0 (5)
N2—Cd2—Cl3ⁱⁱ	92.46 (12)	N7—N8—H8A	108.00
N2ⁱⁱ—Cd2—Cl1	97.50 (11)	N7—N8—H8B	97.00
N2—Cd2—Cl1	82.50 (11)	H8A—N8—H8B	121.00
Cl3—Cd2—Cl1	86.85 (5)	N1—C1—N3	109.7 (5)
Cl3ⁱⁱ—Cd2—Cl1	93.15 (5)	N1—C1—H1	125.2
N2ⁱⁱ—Cd2—Cl1ⁱⁱ	82.50 (11)	N3—C1—H1	125.2
N2—Cd2—Cl1ⁱⁱ	97.50 (11)	N2—C2—N3	109.7 (5)
Cl3—Cd2—Cl1ⁱⁱ	93.15 (5)	N2—C2—H2	125.1
Cl3ⁱⁱ—Cd2—Cl1ⁱⁱ	86.85 (5)	N3—C2—H2	125.1
Cd2—Cl1—Cd1	85.79 (4)	N5—C3—N7	107.6 (5)
Cd1—Cl2—Cd1ⁱⁱⁱ	146.79 (5)	N5—C3—H3	126.2
Cd2—Cl3—Cd1	87.44 (4)	N7—C3—H3	126.2
C1—N1—N2	107.0 (4)	N6—C4—N7	111.1 (6)
C1—N1—Cd1	130.5 (3)	N6—C4—H4	126 (4)
N2—N1—Cd1	120.0 (3)	N7—C4—H4	122 (4)
C2—N2—N1	107.2 (4)	HW2—O1W—HW1	106 (3)
C2—N2—Cd2	136.6 (4)

Symmetry codes: (i) x, −y+1/2, z−1/2; (ii) −x+1, −y+1, −z+1; (iii) x, −y+1/2, z+1/2.

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O1Wⁱⁱ—HW2ⁱⁱ···Cl1	0.86 (6)	2.68 (7)	3.239 (6)	124 (6)
N4^iv—H4B^iv···Cl3	1.00 (8)	2.60 (7)	3.399 (5)	136 (5)
N8^v—H8A^v···Cl2	0.85	2.64	3.370 (5)	144
O1Wⁱⁱ—HW1ⁱⁱ···Cl4	0.86 (7)	2.67 (8)	3.319 (6)	134 (8)
N8—H8B···Cl4	0.90	2.53	3.423 (5)	172
N5^vi—H5^vi···O1W	0.75 (8)	1.97 (8)	2.649 (8)	151 (8)
O1W—HW2···N4ⁱⁱⁱ	0.86 (6)	2.44 (6)	3.247 (9)	157 (6)

Symmetry codes: (ii) −x+1, −y+1, −z+1; (iii) x, −y+1/2, z+1/2; (iv) −x+1, y+1/2, −z+3/2; (v) x, y, z+1; (vi) x−1, −y+1/2, z+1/2.

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