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In the mol­ecule of the title complex, [Zn2(N3)4(C12H10N4)2], each ZnII ion has a distorted tetra­hedral geometry formed by two imidazolyl N atoms and two azide N atoms. Two ZnII ions are bridged by a pair of 1,3-bis­(imidazol-1-yl)benzene ligands, resulting in a macrocyclic complex, located across an inversion center.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806047313/xu2146sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536806047313/xu2146Isup2.hkl
Contains datablock I

CCDC reference: 630514

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](C-C) = 0.005 Å
  • R factor = 0.037
  • wR factor = 0.138
  • Data-to-parameter ratio = 12.4

checkCIF/PLATON results

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Alert level C PLAT220_ALERT_2_C Large Non-Solvent N Ueq(max)/Ueq(min) ... 2.76 Ratio PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for N5 PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for N8 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for Zn PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for N6 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for N9
Alert level G PLAT199_ALERT_1_G Check the Reported _cell_measurement_temperature 293 K PLAT200_ALERT_1_G Check the Reported _diffrn_ambient_temperature . 293 K
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 6 ALERT level C = Check and explain 2 ALERT level G = General alerts; check 2 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 0 ALERT type 3 Indicator that the structure quality may be low 0 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check

Computing details top

Data collection: SMART (Bruker, 2000); cell refinement: SAINT (Bruker, 2000); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Sheldrick, 2000); software used to prepare material for publication: SHELXTL.

Bis[µ-1,3-bis(imidazol-1-yl)benzene-κ2N3:N3']bis[diazidozinc(II)] top
Crystal data top
[Zn2(N3)4(C12H10N4)2]Z = 1
Mr = 719.34F(000) = 364
Triclinic, P1Dx = 1.663 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 7.4056 (9) ÅCell parameters from 2222 reflections
b = 8.9749 (10) Åθ = 2.3–27.6°
c = 11.4207 (13) ŵ = 1.73 mm1
α = 93.867 (2)°T = 293 K
β = 105.193 (2)°Block, colorless
γ = 99.152 (2)°0.34 × 0.25 × 0.19 mm
V = 718.46 (14) Å3
Data collection top
Bruker SMART APEX CCD area-detector
diffractometer
2574 independent reflections
Radiation source: fine-focus sealed tube2267 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.046
φ and ω scansθmax = 25.3°, θmin = 1.8°
Absorption correction: multi-scan
(SADABS; Sheldrick, 2003)
h = 88
Tmin = 0.572, Tmax = 0.730k = 1010
3728 measured reflectionsl = 139
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.037Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.138H-atom parameters constrained
S = 1.22 w = 1/[σ2(Fo2) + (0.0795P)2]
where P = (Fo2 + 2Fc2)/3
2574 reflections(Δ/σ)max = 0.001
208 parametersΔρmax = 0.51 e Å3
0 restraintsΔρmin = 0.51 e Å3
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
xyzUiso*/Ueq
Zn0.69891 (6)0.84854 (4)0.70653 (4)0.0361 (2)
N10.7275 (4)0.8897 (3)0.5413 (3)0.0364 (7)
N20.7581 (4)0.8499 (3)0.3567 (3)0.0323 (7)
N30.9009 (4)0.4132 (3)0.1487 (3)0.0332 (7)
N41.0819 (4)0.2478 (4)0.2092 (3)0.0372 (7)
N50.4687 (6)0.7009 (5)0.6942 (4)0.0593 (11)
N60.3528 (6)0.6434 (4)0.6034 (3)0.0508 (9)
N70.2380 (8)0.5827 (5)0.5179 (5)0.0895 (17)
N80.7230 (7)1.0332 (4)0.8108 (3)0.0598 (11)
N90.7140 (5)1.1595 (4)0.7806 (3)0.0413 (8)
N100.7034 (6)1.2797 (5)0.7579 (4)0.0618 (11)
C10.7326 (6)0.7866 (4)0.4559 (3)0.0392 (9)
H10.72010.68310.46300.047*
C20.7518 (6)1.0268 (4)0.4941 (4)0.0397 (9)
H20.75541.12110.53480.048*
C30.7694 (6)1.0038 (4)0.3814 (4)0.0413 (9)
H30.78591.07730.32960.050*
C40.7609 (5)0.7649 (4)0.2455 (3)0.0327 (8)
C50.6804 (5)0.8152 (5)0.1345 (3)0.0400 (9)
H50.63000.90390.13170.048*
C60.6771 (6)0.7302 (5)0.0287 (4)0.0412 (9)
H60.62600.76340.04620.049*
C70.7484 (5)0.5961 (5)0.0315 (3)0.0399 (9)
H70.74320.53830.04040.048*
C80.8269 (5)0.5509 (4)0.1437 (3)0.0324 (8)
C90.8363 (5)0.6363 (4)0.2517 (3)0.0345 (8)
H90.89300.60600.32690.041*
C101.0534 (5)0.3855 (4)0.2320 (3)0.0351 (8)
H101.12870.45500.29730.042*
C110.8296 (6)0.2854 (5)0.0684 (4)0.0420 (9)
H110.72410.27140.00050.050*
C120.9406 (5)0.1831 (4)0.1058 (4)0.0408 (9)
H120.92450.08490.06810.049*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Zn0.0466 (3)0.0312 (3)0.0303 (3)0.0095 (2)0.0097 (2)0.00105 (18)
N10.0450 (18)0.0329 (17)0.0310 (16)0.0085 (14)0.0094 (14)0.0018 (13)
N20.0389 (16)0.0300 (16)0.0302 (16)0.0103 (13)0.0102 (13)0.0061 (12)
N30.0354 (16)0.0371 (18)0.0265 (15)0.0075 (13)0.0079 (13)0.0001 (13)
N40.0443 (18)0.0357 (17)0.0307 (16)0.0087 (14)0.0087 (14)0.0018 (13)
N50.062 (2)0.059 (3)0.049 (2)0.007 (2)0.010 (2)0.0135 (19)
N60.060 (2)0.037 (2)0.052 (2)0.0005 (17)0.013 (2)0.0162 (17)
N70.108 (4)0.055 (3)0.068 (3)0.025 (3)0.017 (3)0.013 (2)
N80.097 (3)0.040 (2)0.041 (2)0.027 (2)0.011 (2)0.0052 (16)
N90.0421 (19)0.040 (2)0.0401 (19)0.0083 (15)0.0099 (15)0.0052 (15)
N100.066 (3)0.052 (3)0.069 (3)0.010 (2)0.022 (2)0.011 (2)
C10.050 (2)0.035 (2)0.034 (2)0.0101 (17)0.0126 (17)0.0065 (17)
C20.053 (2)0.0249 (19)0.045 (2)0.0148 (17)0.0155 (19)0.0054 (16)
C30.050 (2)0.034 (2)0.045 (2)0.0136 (17)0.0163 (19)0.0132 (17)
C40.0318 (17)0.037 (2)0.0306 (19)0.0055 (15)0.0107 (15)0.0049 (15)
C50.037 (2)0.053 (2)0.037 (2)0.0169 (18)0.0139 (17)0.0177 (18)
C60.044 (2)0.054 (2)0.031 (2)0.0184 (18)0.0122 (17)0.0165 (18)
C70.039 (2)0.057 (3)0.0273 (19)0.0140 (18)0.0119 (16)0.0059 (17)
C80.0302 (17)0.0334 (19)0.0340 (19)0.0070 (14)0.0092 (15)0.0034 (15)
C90.0350 (19)0.044 (2)0.0251 (18)0.0098 (16)0.0064 (15)0.0079 (15)
C100.042 (2)0.0294 (19)0.0300 (19)0.0063 (15)0.0054 (16)0.0014 (15)
C110.036 (2)0.049 (2)0.035 (2)0.0056 (18)0.0047 (16)0.0085 (18)
C120.043 (2)0.034 (2)0.042 (2)0.0036 (17)0.0124 (18)0.0094 (17)
Geometric parameters (Å, º) top
Zn—N12.005 (3)C1—H10.9300
Zn—N4i2.012 (3)C2—C31.333 (6)
Zn—N51.953 (4)C2—H20.9300
Zn—N81.930 (4)C3—H30.9300
N1—C11.311 (5)C4—C91.358 (5)
N1—C21.382 (5)C4—C51.390 (5)
N2—C11.344 (5)C5—C61.377 (6)
N2—C31.375 (5)C5—H50.9300
N2—C41.444 (5)C6—C71.388 (6)
N3—C101.342 (5)C6—H60.9300
N3—C111.359 (5)C7—C81.379 (5)
N3—C81.428 (5)C7—H70.9300
N4—C101.307 (5)C8—C91.387 (5)
N4—C121.375 (5)C9—H90.9300
N5—N61.183 (5)C10—H100.9300
N6—N71.148 (5)C11—C121.346 (6)
N8—N91.214 (5)C11—H110.9300
N9—N101.136 (5)C12—H120.9300
N8—Zn—N5113.8 (2)C2—C3—H3126.7
N8—Zn—N1112.16 (15)N2—C3—H3126.7
N5—Zn—N1111.59 (15)C9—C4—C5121.9 (4)
N8—Zn—N4i104.78 (15)C9—C4—N2119.4 (3)
N5—Zn—N4i105.99 (15)C5—C4—N2118.6 (3)
N1—Zn—N4i107.95 (13)C6—C5—C4118.2 (4)
C1—N1—C2105.6 (3)C6—C5—H5120.9
C1—N1—Zn125.2 (3)C4—C5—H5120.9
C2—N1—Zn129.1 (3)C5—C6—C7121.4 (4)
C1—N2—C3106.9 (3)C5—C6—H6119.3
C1—N2—C4124.2 (3)C7—C6—H6119.3
C3—N2—C4128.8 (3)C8—C7—C6118.2 (4)
C10—N3—C11107.1 (3)C8—C7—H7120.9
C10—N3—C8126.9 (3)C6—C7—H7120.9
C11—N3—C8126.0 (3)C7—C8—C9121.6 (4)
C10—N4—C12106.3 (3)C7—C8—N3119.1 (3)
C10—N4—Zni128.3 (3)C9—C8—N3119.3 (3)
C12—N4—Zni125.1 (3)C4—C9—C8118.6 (3)
N6—N5—Zn126.7 (3)C4—C9—H9120.7
N7—N6—N5177.1 (5)C8—C9—H9120.7
N9—N8—Zn127.5 (3)N4—C10—N3111.0 (3)
N10—N9—N8176.4 (4)N4—C10—H10124.5
N1—C1—N2111.2 (3)N3—C10—H10124.5
N1—C1—H1124.4C12—C11—N3106.9 (3)
N2—C1—H1124.4C12—C11—H11126.5
C3—C2—N1109.7 (3)N3—C11—H11126.5
C3—C2—H2125.1C11—C12—N4108.7 (3)
N1—C2—H2125.1C11—C12—H12125.7
C2—C3—N2106.5 (3)N4—C12—H12125.7
N8—Zn—N1—C1174.3 (3)C3—N2—C4—C533.0 (5)
N5—Zn—N1—C156.7 (4)C9—C4—C5—C60.4 (6)
N4i—Zn—N1—C159.4 (4)N2—C4—C5—C6177.5 (3)
N8—Zn—N1—C23.3 (4)C4—C5—C6—C71.3 (6)
N5—Zn—N1—C2125.7 (3)C5—C6—C7—C81.3 (6)
N4i—Zn—N1—C2118.2 (3)C6—C7—C8—C90.3 (6)
N8—Zn—N5—N6125.7 (4)C6—C7—C8—N3179.9 (3)
N1—Zn—N5—N62.4 (5)C10—N3—C8—C7144.8 (4)
N4i—Zn—N5—N6119.7 (4)C11—N3—C8—C734.7 (5)
N5—Zn—N8—N9111.9 (4)C10—N3—C8—C935.0 (5)
N1—Zn—N8—N915.9 (5)C11—N3—C8—C9145.5 (4)
N4i—Zn—N8—N9132.8 (4)C5—C4—C9—C81.9 (6)
C2—N1—C1—N20.2 (5)N2—C4—C9—C8176.0 (3)
Zn—N1—C1—N2178.3 (2)C7—C8—C9—C41.9 (6)
C3—N2—C1—N10.2 (5)N3—C8—C9—C4178.3 (3)
C4—N2—C1—N1177.0 (3)C12—N4—C10—N30.0 (4)
C1—N1—C2—C30.5 (5)Zni—N4—C10—N3173.8 (2)
Zn—N1—C2—C3178.5 (3)C11—N3—C10—N40.2 (4)
N1—C2—C3—N20.6 (5)C8—N3—C10—N4179.8 (3)
C1—N2—C3—C20.5 (4)C10—N3—C11—C120.3 (4)
C4—N2—C3—C2177.1 (3)C8—N3—C11—C12179.9 (3)
C1—N2—C4—C934.8 (5)N3—C11—C12—N40.4 (5)
C3—N2—C4—C9149.0 (4)C10—N4—C12—C110.2 (4)
C1—N2—C4—C5143.1 (4)Zni—N4—C12—C11173.9 (3)
Symmetry code: (i) x+2, y+1, z+1.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
C1—H1···N7ii0.932.473.384 (6)167
C10—H10···N7iii0.932.563.431 (6)156
C11—H11···N9iv0.932.623.245 (6)125
Symmetry codes: (ii) x+1, y+1, z+1; (iii) x+1, y, z; (iv) x, y1, z1.
 

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