Poly[(nitrato-κO)tris(μ3-1H-1,2,4-triazolato)dizinc(II)]: a three-dimensional coordination polymer
Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807049574/hb2547sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536807049574/hb2547Isup2.hkl |
CCDC reference: 667171
Key indicators
- Single-crystal X-ray study
- T = 150 K
- Mean (N-C) = 0.003 Å
- Disorder in main residue
- R factor = 0.024
- wR factor = 0.062
- Data-to-parameter ratio = 13.5
checkCIF/PLATON results
No syntax errors found
Alert level C ABSTM02_ALERT_3_C The ratio of expected to reported Tmax/Tmin(RR) is > 1.10 Tmin and Tmax reported: 0.808 1.000 Tmin and Tmax expected: 0.306 0.449 RR = 1.184 Please check that your absorption correction is appropriate. PLAT060_ALERT_3_C Ratio Tmax/Tmin (Exp-to-Rep) (too) Large ....... 1.18 PLAT062_ALERT_4_C Rescale T(min) & T(max) by ..................... 0.45 PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for O2A PLAT301_ALERT_3_C Main Residue Disorder ......................... 14.00 Perc. PLAT313_ALERT_2_C Oxygen with three covalent bonds (rare) ........ O2B PLAT313_ALERT_2_C Oxygen with three covalent bonds (rare) ........ O3B
Alert level G ABSTM02_ALERT_3_G When printed, the submitted absorption T values will be replaced by the scaled T values. Since the ratio of scaled T's is identical to the ratio of reported T values, the scaling does not imply a change to the absorption corrections used in the study. Ratio of Tmax expected/reported 0.449 Tmax scaled 0.449 Tmin scaled 0.363 PLAT860_ALERT_3_G Note: Number of Least-Squares Restraints ....... 3
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 7 ALERT level C = Check and explain 2 ALERT level G = General alerts; check 0 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 5 ALERT type 3 Indicator that the structure quality may be low 1 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check
For the isostructural Co phase, see: Ouellette et al. (2006). For related literature, see: Goforth et al. (2005); Su et al. (2004).
In a typical procedure trz (0.5 mmol) and Zn(NO3)2 (0.5 mmol) were weighed and placed in a 23 ml Teflon lined autoclave together with 5 ml water and 5 ml e thanol, which functioned as the reaction solvent. The autoclave was subsequently sealed and heated at a rate of 1 K/min to 433 K. The temperature was held at 433 K for three days before it was decreased, at a rate of 0.1 K/min, to 353 K where it was then held for 6 h. Finally, the temperature was decreased at a rate of 0.1 K/min to room temperature. Colorless blocks of (I) were hand picked from the reaction and used for single-crystal analyses.
The atoms of the minor nitrate disorder component were refined with Uiso values. The hydrogen atoms were placed in geometrically idealized positions and included as riding atoms. The final difference map extrema are +0.84 e-/Å3 (0.98 Å from Zn1) and -0.52 e-/Å3 (0.51 Å from O1B).
The title compound, (I), was solvothermally synthesized from Zn(NO3)2 and 1,2,4–1H-triazole (Htrz) in a 1:1 molar ratio in an ethanol/water solvent mixture. Single crystal X-ray analysis determined that the transparent crystals contain a complicated three-dimensional atomic network whose asymmetric unit is shown in Figure 1. There are two crystallographically distinct Zn centers (Figure 2). Zn1 atoms are in a tetrahedral coordination sphere, coordinated to three trz ligands and one disordered NO3. Zn2 atoms are in an octahedral coordination sphere, coordinated to six trz ligands (Figure 2 b). The nitrate anion coordinated to Zn1 is disordered over two independent positions in the asymmetric unit, and three positions when the mirror symmetry of the crystal is taken into account, in the proportion 40/40/20 (Figure 2a). Each Zn center forms its own one-dimensional chain/column along the a axis through the anionic bridging mode of the trz ligands, whose connectives generate a three-dimensional structure (Figure 3). Zn2 and its ligands form infinite one-dimensional chains down the a axis. These one-dimensional chains propagate by the N1,N2 bridging mode (see Figure 4) of the trz ligands. Each Zn2 one-dimensional chain is bridged via a N4 mode to columns of tetrahedrally coordinated Zn1 atoms. The Zn—O and Zn—N bond distances (Table 1) are comparable to those in an isostructural complex synthesized with Co (Ouellette et al., 2006). Additionally, the bridging characteristics of trz in [Zn2(trz)3(NO3)] are similar to our previous work involving trz and ZnF, in that all trz ring nitrogen atoms coordinate to the Zn centers through an N1,N2,N4 bridging mode (Goforth et al., 2005; Su et al., 2004).
For the isostructural Co phase, see: Ouellette et al. (2006). For related literature, see: Goforth et al. (2005); Su et al. (2004).
Data collection: SMART (Bruker, 2001); cell refinement: SAINT-Plus (Bruker, 2001); data reduction: SAINT-Plus (Bruker, 2001); program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: various; software used to prepare material for publication: SHELXTL (Bruker, 2000).
[Zn2(C2H2N3)3(NO3)] | F(000) = 784 |
Mr = 396.95 | Dx = 1.986 Mg m−3 |
Orthorhombic, Pnma | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ac 2n | Cell parameters from 5133 reflections |
a = 7.6001 (4) Å | θ = 2.4–28.3° |
b = 9.9758 (5) Å | µ = 3.64 mm−1 |
c = 17.5108 (8) Å | T = 150 K |
V = 1327.62 (11) Å3 | Block, colorless |
Z = 4 | 0.36 × 0.28 × 0.22 mm |
Bruker SMART APEX CCD diffractometer | 1752 independent reflections |
Radiation source: fine-focus sealed tube | 1627 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.037 |
ω scans | θmax = 28.3°, θmin = 2.3° |
Absorption correction: multi-scan (SADABS; Bruker, 2001) | h = −10→10 |
Tmin = 0.808, Tmax = 1.000 | k = −13→13 |
12217 measured reflections | l = −22→23 |
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.025 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.062 | H-atom parameters constrained |
S = 1.08 | w = 1/[σ2(Fo2) + (0.0321P)2 + 0.8204P] where P = (Fo2 + 2Fc2)/3 |
1752 reflections | (Δ/σ)max = 0.001 |
130 parameters | Δρmax = 0.84 e Å−3 |
3 restraints | Δρmin = −0.52 e Å−3 |
[Zn2(C2H2N3)3(NO3)] | V = 1327.62 (11) Å3 |
Mr = 396.95 | Z = 4 |
Orthorhombic, Pnma | Mo Kα radiation |
a = 7.6001 (4) Å | µ = 3.64 mm−1 |
b = 9.9758 (5) Å | T = 150 K |
c = 17.5108 (8) Å | 0.36 × 0.28 × 0.22 mm |
Bruker SMART APEX CCD diffractometer | 1752 independent reflections |
Absorption correction: multi-scan (SADABS; Bruker, 2001) | 1627 reflections with I > 2σ(I) |
Tmin = 0.808, Tmax = 1.000 | Rint = 0.037 |
12217 measured reflections |
R[F2 > 2σ(F2)] = 0.025 | 3 restraints |
wR(F2) = 0.062 | H-atom parameters constrained |
S = 1.08 | Δρmax = 0.84 e Å−3 |
1752 reflections | Δρmin = −0.52 e Å−3 |
130 parameters |
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. |
x | y | z | Uiso*/Ueq | Occ. (<1) | |
Zn1 | 0.65025 (4) | 0.7500 | 0.580742 (16) | 0.01318 (10) | |
Zn2 | 0.51023 (3) | 0.7500 | 0.237037 (17) | 0.01112 (9) | |
C1 | 0.5883 (3) | 0.7500 | 0.41412 (15) | 0.0190 (6) | |
H1 | 0.4647 | 0.7500 | 0.4223 | 0.023* | |
C2 | 0.8619 (3) | 0.7500 | 0.43286 (16) | 0.0187 (5) | |
H2 | 0.9738 | 0.7500 | 0.4571 | 0.022* | |
C3 | 0.5824 (2) | 0.51411 (19) | 0.67750 (11) | 0.0180 (4) | |
H3 | 0.4628 | 0.5408 | 0.6816 | 0.022* | |
C4 | 0.8505 (2) | 0.5094 (2) | 0.64855 (11) | 0.0180 (4) | |
H4 | 0.9621 | 0.5317 | 0.6277 | 0.022* | |
N1 | 0.7073 (3) | 0.7500 | 0.47113 (13) | 0.0161 (4) | |
N2 | 0.6611 (3) | 0.7500 | 0.34565 (13) | 0.0157 (4) | |
N3 | 0.8397 (3) | 0.7500 | 0.35800 (13) | 0.0156 (4) | |
N4 | 0.7043 (2) | 0.58402 (15) | 0.63830 (9) | 0.0158 (3) | |
N5 | 0.64612 (18) | 0.40513 (15) | 0.70959 (9) | 0.0149 (3) | |
N6 | 0.82168 (19) | 0.40187 (15) | 0.69069 (9) | 0.0147 (3) | |
N7A | 0.2668 (6) | 0.7091 (4) | 0.5694 (2) | 0.0247 (11) | 0.40 |
O1A | 0.3900 (4) | 0.7852 (3) | 0.5936 (2) | 0.0270 (10) | 0.40 |
O2A | 0.3091 (7) | 0.6066 (5) | 0.5355 (3) | 0.0520 (13) | 0.40 |
O3A | 0.1108 (3) | 0.7500 | 0.58235 (14) | 0.0383 (6) | 0.80 |
N7B | 0.2657 (13) | 0.7500 | 0.6055 (6) | 0.029 (3)* | 0.20 |
O1B | 0.3885 (15) | 0.7500 | 0.5567 (7) | 0.026 (3)* | 0.20 |
O2B | 0.3006 (15) | 0.7500 | 0.6737 (6) | 0.033 (3)* | 0.20 |
O3B | 0.1108 (3) | 0.7500 | 0.58235 (14) | 0.0383 (6) | 0.20 |
U11 | U22 | U33 | U12 | U13 | U23 | |
Zn1 | 0.01843 (17) | 0.01104 (16) | 0.01007 (16) | 0.000 | 0.00027 (10) | 0.000 |
Zn2 | 0.00955 (15) | 0.01216 (16) | 0.01165 (17) | 0.000 | 0.00029 (9) | 0.000 |
C1 | 0.0141 (12) | 0.0284 (15) | 0.0145 (13) | 0.000 | 0.0019 (9) | 0.000 |
C2 | 0.0138 (11) | 0.0277 (15) | 0.0146 (13) | 0.000 | −0.0020 (9) | 0.000 |
C3 | 0.0145 (8) | 0.0166 (9) | 0.0229 (10) | 0.0028 (7) | 0.0014 (7) | 0.0048 (8) |
C4 | 0.0160 (8) | 0.0179 (9) | 0.0201 (10) | −0.0005 (7) | 0.0029 (7) | 0.0052 (8) |
N1 | 0.0179 (10) | 0.0191 (11) | 0.0114 (10) | 0.000 | −0.0003 (8) | 0.000 |
N2 | 0.0121 (10) | 0.0237 (12) | 0.0114 (10) | 0.000 | 0.0001 (8) | 0.000 |
N3 | 0.0123 (10) | 0.0201 (11) | 0.0143 (11) | 0.000 | 0.0002 (8) | 0.000 |
N4 | 0.0181 (7) | 0.0137 (8) | 0.0155 (8) | 0.0009 (6) | −0.0004 (6) | 0.0013 (6) |
N5 | 0.0117 (7) | 0.0152 (8) | 0.0179 (8) | 0.0008 (5) | 0.0008 (6) | 0.0032 (6) |
N6 | 0.0121 (7) | 0.0157 (8) | 0.0164 (8) | −0.0002 (5) | 0.0004 (5) | 0.0022 (6) |
N7A | 0.030 (2) | 0.027 (3) | 0.018 (2) | −0.0082 (16) | −0.0016 (17) | 0.0046 (17) |
O1A | 0.0148 (16) | 0.026 (3) | 0.040 (2) | −0.0033 (12) | −0.0037 (15) | −0.0135 (16) |
O2A | 0.047 (3) | 0.039 (3) | 0.070 (4) | −0.009 (2) | −0.002 (3) | −0.029 (3) |
O3A | 0.0173 (10) | 0.0551 (17) | 0.0425 (15) | 0.000 | −0.0022 (10) | 0.000 |
O3B | 0.0173 (10) | 0.0551 (17) | 0.0425 (15) | 0.000 | −0.0022 (10) | 0.000 |
Zn1—N1 | 1.968 (2) | C3—N5 | 1.316 (2) |
Zn1—N4i | 1.9814 (16) | C3—N4 | 1.348 (2) |
Zn1—N4 | 1.9815 (15) | C3—H3 | 0.9500 |
Zn1—O1Ai | 2.021 (4) | C4—N6 | 1.320 (2) |
Zn1—O1A | 2.021 (4) | C4—N4 | 1.349 (2) |
Zn1—O1B | 2.033 (12) | C4—H4 | 0.9500 |
Zn2—N3ii | 2.109 (2) | N2—N3 | 1.375 (3) |
Zn2—N6iii | 2.1415 (15) | N3—Zn2vii | 2.109 (2) |
Zn2—N6iv | 2.1415 (15) | N5—N6 | 1.375 (2) |
Zn2—N5v | 2.1634 (15) | N5—Zn2vi | 2.1635 (15) |
Zn2—N5vi | 2.1635 (15) | N6—Zn2viii | 2.1415 (15) |
Zn2—N2 | 2.221 (2) | N7A—O2A | 1.225 (6) |
C1—N2 | 1.321 (3) | N7A—O3A | 1.274 (5) |
C1—N1 | 1.347 (3) | N7A—O1A | 1.277 (5) |
C1—H1 | 0.9500 | O3A—N7Ai | 1.274 (5) |
C2—N3 | 1.322 (3) | N7B—O2B | 1.222 (11) |
C2—N1 | 1.353 (3) | N7B—O1B | 1.266 (11) |
C2—H2 | 0.9500 | ||
N1—Zn1—N4i | 116.77 (5) | C1—N1—C2 | 102.5 (2) |
N1—Zn1—N4 | 116.77 (5) | C1—N1—Zn1 | 125.11 (18) |
N4i—Zn1—N4 | 113.36 (9) | C2—N1—Zn1 | 132.41 (19) |
N1—Zn1—O1Ai | 108.90 (13) | C1—N2—N3 | 105.7 (2) |
N4i—Zn1—O1Ai | 106.94 (11) | C1—N2—Zn2 | 124.16 (17) |
N4—Zn1—O1Ai | 90.08 (11) | N3—N2—Zn2 | 130.14 (17) |
N1—Zn1—O1A | 108.90 (13) | C2—N3—N2 | 106.4 (2) |
N4i—Zn1—O1A | 90.08 (11) | C2—N3—Zn2vii | 134.77 (17) |
N4—Zn1—O1A | 106.94 (12) | N2—N3—Zn2vii | 118.86 (17) |
N1—Zn1—O1B | 90.8 (3) | C3—N4—C4 | 102.28 (15) |
N4i—Zn1—O1B | 107.94 (17) | C3—N4—Zn1 | 123.29 (12) |
N4—Zn1—O1B | 107.94 (17) | C4—N4—Zn1 | 134.40 (13) |
N3ii—Zn2—N6iii | 93.87 (6) | C3—N5—N6 | 105.90 (15) |
N3ii—Zn2—N6iv | 93.87 (6) | C3—N5—Zn2vi | 124.97 (12) |
N6iii—Zn2—N6iv | 90.06 (8) | N6—N5—Zn2vi | 128.32 (11) |
N3ii—Zn2—N5v | 90.20 (6) | C4—N6—N5 | 106.04 (14) |
N6iii—Zn2—N5v | 89.16 (6) | C4—N6—Zn2viii | 133.44 (12) |
N6iv—Zn2—N5v | 175.90 (6) | N5—N6—Zn2viii | 120.29 (11) |
N3ii—Zn2—N5vi | 90.20 (6) | N7Ai—N7A—O1Ai | 86.8 (3) |
N6iii—Zn2—N5vi | 175.90 (6) | N7Ai—N7A—O2A | 146.6 (3) |
N6iv—Zn2—N5vi | 89.16 (6) | O1Ai—N7A—O2A | 90.4 (4) |
N5v—Zn2—N5vi | 91.34 (8) | N7Ai—N7A—O3A | 71.34 (19) |
N3ii—Zn2—N2 | 173.18 (8) | O1Ai—N7A—O3A | 139.1 (5) |
N6iii—Zn2—N2 | 90.95 (6) | O2A—N7A—O3A | 126.7 (4) |
N6iv—Zn2—N2 | 90.95 (6) | N7Ai—N7A—O1A | 53.6 (3) |
N5v—Zn2—N2 | 85.04 (6) | O2A—N7A—O1A | 117.6 (4) |
N5vi—Zn2—N2 | 85.04 (6) | O3A—N7A—O1A | 115.7 (4) |
N2—C1—N1 | 113.1 (2) | O1Ai—O1A—N7Ai | 93.2 (3) |
N2—C1—H1 | 123.5 | O1Ai—O1A—N7A | 53.6 (3) |
N1—C1—H1 | 123.5 | O1Ai—O1A—O2Ai | 132.2 (3) |
N3—C2—N1 | 112.4 (2) | N7Ai—O1A—O2Ai | 49.7 (3) |
N3—C2—H2 | 123.8 | N7A—O1A—O2Ai | 84.7 (3) |
N1—C2—H2 | 123.8 | O1Ai—O1A—Zn1 | 80.01 (10) |
N5—C3—N4 | 113.07 (16) | N7Ai—O1A—Zn1 | 148.6 (4) |
N5—C3—H3 | 123.5 | N7A—O1A—Zn1 | 125.3 (3) |
N4—C3—H3 | 123.5 | O2Ai—O1A—Zn1 | 114.9 (3) |
N6—C4—N4 | 112.71 (16) | O2B—N7B—O1B | 119.9 (12) |
N6—C4—H4 | 123.6 | N7B—O1B—Zn1 | 125.6 (10) |
N4—C4—H4 | 123.6 | ||
N2—C1—N1—C2 | 0.0 | Zn2vi—N5—N6—C4 | 169.93 (14) |
N2—C1—N1—Zn1 | 180.0 | C3—N5—N6—Zn2viii | 175.21 (12) |
N3—C2—N1—C1 | 0.0 | Zn2vi—N5—N6—Zn2viii | −14.9 (2) |
N3—C2—N1—Zn1 | 180.0 | N7Ai—N7A—O1A—O1Ai | −179.988 (2) |
N4i—Zn1—N1—C1 | −110.62 (6) | O2A—N7A—O1A—O1Ai | −38.3 (4) |
N4—Zn1—N1—C1 | 110.62 (6) | O3A—N7A—O1A—O1Ai | 142.7 (5) |
O1Ai—Zn1—N1—C1 | 10.57 (10) | O1Ai—N7A—O1A—N7Ai | 180.0 |
O1A—Zn1—N1—C1 | −10.57 (10) | O2A—N7A—O1A—N7Ai | 141.7 (4) |
O1B—Zn1—N1—C1 | 0.0 | O3A—N7A—O1A—N7Ai | −37.3 (5) |
N4i—Zn1—N1—C2 | 69.38 (6) | N7Ai—N7A—O1A—O2Ai | −24.9 (3) |
N4—Zn1—N1—C2 | −69.38 (6) | O1Ai—N7A—O1A—O2Ai | 155.1 (3) |
O1Ai—Zn1—N1—C2 | −169.43 (10) | O2A—N7A—O1A—O2Ai | 116.8 (6) |
O1A—Zn1—N1—C2 | 169.43 (10) | O3A—N7A—O1A—O2Ai | −62.2 (4) |
O1B—Zn1—N1—C2 | 180.0 | N7Ai—N7A—O1A—Zn1 | −141.8 (5) |
N1—C1—N2—N3 | 0.000 (1) | O1Ai—N7A—O1A—Zn1 | 38.2 (5) |
N1—C1—N2—Zn2 | 180.0 | O2A—N7A—O1A—Zn1 | −0.2 (7) |
N6iii—Zn2—N2—C1 | 134.96 (4) | O3A—N7A—O1A—Zn1 | −179.1 (3) |
N6iv—Zn2—N2—C1 | −134.96 (4) | N1—Zn1—O1A—O1Ai | 93.45 (4) |
N5v—Zn2—N2—C1 | 45.89 (4) | N4i—Zn1—O1A—O1Ai | −148.08 (5) |
N5vi—Zn2—N2—C1 | −45.89 (4) | N4—Zn1—O1A—O1Ai | −33.57 (5) |
N6iii—Zn2—N2—N3 | −45.04 (4) | O1B—Zn1—O1A—O1Ai | 62.5 (6) |
N6iv—Zn2—N2—N3 | 45.04 (4) | N1—Zn1—O1A—N7Ai | 13.9 (7) |
N5v—Zn2—N2—N3 | −134.11 (4) | N4i—Zn1—O1A—N7Ai | 132.4 (7) |
N5vi—Zn2—N2—N3 | 134.11 (4) | N4—Zn1—O1A—N7Ai | −113.1 (7) |
N1—C2—N3—N2 | 0.0 | O1Ai—Zn1—O1A—N7Ai | −79.6 (7) |
N1—C2—N3—Zn2vii | 180.0 | O1B—Zn1—O1A—N7Ai | −17.1 (6) |
C1—N2—N3—C2 | 0.000 (1) | N1—Zn1—O1A—N7A | 63.1 (4) |
Zn2—N2—N3—C2 | 180.0 | N4i—Zn1—O1A—N7A | −178.4 (4) |
C1—N2—N3—Zn2vii | 180.0 | N4—Zn1—O1A—N7A | −63.9 (4) |
Zn2—N2—N3—Zn2vii | 0.0 | O1Ai—Zn1—O1A—N7A | −30.3 (4) |
N5—C3—N4—C4 | 0.0 (2) | O1B—Zn1—O1A—N7A | 32.1 (6) |
N5—C3—N4—Zn1 | 178.11 (13) | N1—Zn1—O1A—O2Ai | −38.7 (3) |
N6—C4—N4—C3 | 0.0 (2) | N4i—Zn1—O1A—O2Ai | 79.8 (3) |
N6—C4—N4—Zn1 | −177.80 (14) | N4—Zn1—O1A—O2Ai | −165.7 (3) |
N1—Zn1—N4—C3 | −122.50 (16) | O1Ai—Zn1—O1A—O2Ai | −132.1 (3) |
N4i—Zn1—N4—C3 | 97.36 (16) | O1B—Zn1—O1A—O2Ai | −69.6 (6) |
O1Ai—Zn1—N4—C3 | −11.19 (19) | N7Ai—N7A—O2A—O1Ai | 84.9 (6) |
O1A—Zn1—N4—C3 | −0.29 (19) | O3A—N7A—O2A—O1Ai | −161.3 (7) |
O1B—Zn1—N4—C3 | −22.2 (3) | O1A—N7A—O2A—O1Ai | 19.9 (3) |
N1—Zn1—N4—C4 | 54.9 (2) | O1Ai—N7A—O3A—N7Ai | 61.4 (7) |
N4i—Zn1—N4—C4 | −85.2 (2) | O2A—N7A—O3A—N7Ai | −147.9 (5) |
O1Ai—Zn1—N4—C4 | 166.2 (2) | O1A—N7A—O3A—N7Ai | 31.0 (4) |
O1A—Zn1—N4—C4 | 177.1 (2) | O2B—N7B—O1B—Zn1 | 0.000 (4) |
O1B—Zn1—N4—C4 | 155.3 (4) | N1—Zn1—O1B—N7B | 180.000 (3) |
N4—C3—N5—N6 | 0.0 (2) | N4i—Zn1—O1B—N7B | −61.44 (11) |
N4—C3—N5—Zn2vi | −170.37 (13) | N4—Zn1—O1B—N7B | 61.44 (11) |
N4—C4—N6—N5 | 0.0 (2) | O1Ai—Zn1—O1B—N7B | 29.2 (5) |
N4—C4—N6—Zn2viii | −174.30 (13) | O1A—Zn1—O1B—N7B | −29.2 (5) |
C3—N5—N6—C4 | 0.0 (2) |
Symmetry codes: (i) x, −y+3/2, z; (ii) x−1/2, y, −z+1/2; (iii) −x+3/2, y+1/2, z−1/2; (iv) −x+3/2, −y+1, z−1/2; (v) −x+1, y+1/2, −z+1; (vi) −x+1, −y+1, −z+1; (vii) x+1/2, y, −z+1/2; (viii) −x+3/2, −y+1, z+1/2. |
Experimental details
Crystal data | |
Chemical formula | [Zn2(C2H2N3)3(NO3)] |
Mr | 396.95 |
Crystal system, space group | Orthorhombic, Pnma |
Temperature (K) | 150 |
a, b, c (Å) | 7.6001 (4), 9.9758 (5), 17.5108 (8) |
V (Å3) | 1327.62 (11) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 3.64 |
Crystal size (mm) | 0.36 × 0.28 × 0.22 |
Data collection | |
Diffractometer | Bruker SMART APEX CCD |
Absorption correction | Multi-scan (SADABS; Bruker, 2001) |
Tmin, Tmax | 0.808, 1.000 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 12217, 1752, 1627 |
Rint | 0.037 |
(sin θ/λ)max (Å−1) | 0.667 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.025, 0.062, 1.08 |
No. of reflections | 1752 |
No. of parameters | 130 |
No. of restraints | 3 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 0.84, −0.52 |
Computer programs: SMART (Bruker, 2001), SAINT-Plus (Bruker, 2001), SHELXS97 (Sheldrick, 1990), SHELXL97 (Sheldrick, 1997), various, SHELXTL (Bruker, 2000).
Zn1—N1 | 1.968 (2) | Zn2—N3ii | 2.109 (2) |
Zn1—N4i | 1.9814 (16) | Zn2—N6iii | 2.1415 (15) |
Zn1—N4 | 1.9815 (15) | Zn2—N6iv | 2.1415 (15) |
Zn1—O1Ai | 2.021 (4) | Zn2—N5v | 2.1634 (15) |
Zn1—O1A | 2.021 (4) | Zn2—N5vi | 2.1635 (15) |
Zn1—O1B | 2.033 (12) | Zn2—N2 | 2.221 (2) |
Symmetry codes: (i) x, −y+3/2, z; (ii) x−1/2, y, −z+1/2; (iii) −x+3/2, y+1/2, z−1/2; (iv) −x+3/2, −y+1, z−1/2; (v) −x+1, y+1/2, −z+1; (vi) −x+1, −y+1, −z+1. |
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The title compound, (I), was solvothermally synthesized from Zn(NO3)2 and 1,2,4–1H-triazole (Htrz) in a 1:1 molar ratio in an ethanol/water solvent mixture. Single crystal X-ray analysis determined that the transparent crystals contain a complicated three-dimensional atomic network whose asymmetric unit is shown in Figure 1. There are two crystallographically distinct Zn centers (Figure 2). Zn1 atoms are in a tetrahedral coordination sphere, coordinated to three trz ligands and one disordered NO3. Zn2 atoms are in an octahedral coordination sphere, coordinated to six trz ligands (Figure 2 b). The nitrate anion coordinated to Zn1 is disordered over two independent positions in the asymmetric unit, and three positions when the mirror symmetry of the crystal is taken into account, in the proportion 40/40/20 (Figure 2a). Each Zn center forms its own one-dimensional chain/column along the a axis through the anionic bridging mode of the trz ligands, whose connectives generate a three-dimensional structure (Figure 3). Zn2 and its ligands form infinite one-dimensional chains down the a axis. These one-dimensional chains propagate by the N1,N2 bridging mode (see Figure 4) of the trz ligands. Each Zn2 one-dimensional chain is bridged via a N4 mode to columns of tetrahedrally coordinated Zn1 atoms. The Zn—O and Zn—N bond distances (Table 1) are comparable to those in an isostructural complex synthesized with Co (Ouellette et al., 2006). Additionally, the bridging characteristics of trz in [Zn2(trz)3(NO3)] are similar to our previous work involving trz and ZnF, in that all trz ring nitrogen atoms coordinate to the Zn centers through an N1,N2,N4 bridging mode (Goforth et al., 2005; Su et al., 2004).