In the title mononuclear zinc complex, [ZnCl2(C8H7N3)2]·0.5H2O, the Zn atom is located on a twofold axis and has a slightly distorted octahedral geometry consisting of four N atoms from two 2-(2-pyridyl)imidazole ligands and two Cl− anions. The complex molecules are connected through intermolecular hydrogen bonds, forming a two-dimensional layer structure.
Supporting information
CCDC reference: 630011
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (C-C) = 0.003 Å
- Disorder in solvent or counterion
- R factor = 0.028
- wR factor = 0.091
- Data-to-parameter ratio = 17.1
checkCIF/PLATON results
No syntax errors found
Alert level C
PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings Differ .... ?
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ?
PLAT045_ALERT_1_C Calculated and Reported Z Differ by ............ 0.50 Ratio
PLAT062_ALERT_4_C Rescale T(min) & T(max) by ..................... 2.91
PLAT076_ALERT_1_C Occupancy 0.50 less than 1.0 for Sp.pos . O1W
PLAT147_ALERT_1_C su on Symmetry Constrained Cell Angle(s) ....... ?
PLAT302_ALERT_4_C Anion/Solvent Disorder ......................... 50.00 Perc.
Alert level G
FORMU01_ALERT_1_G There is a discrepancy between the atom counts in the
_chemical_formula_sum and _chemical_formula_moiety. This is
usually due to the moiety formula being in the wrong format.
Atom count from _chemical_formula_sum: C16 H15 Cl2 N6 O0.5 Zn1
Atom count from _chemical_formula_moiety:C16 H16 Cl2 N6 O0.5 Zn1
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 2.911
Tmax scaled 0.635 Tmin scaled 0.611
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
7 ALERT level C = Check and explain
4 ALERT level G = General alerts; check
8 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
0 ALERT type 2 Indicator that the structure model may be wrong or deficient
1 ALERT type 3 Indicator that the structure quality may be low
2 ALERT type 4 Improvement, methodology, query or suggestion
0 ALERT type 5 Informative message, check
Data collection: SMART (Bruker, 1997); cell refinement: SAINT (Bruker, 1999); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL-Plus (Sheldrick, 1990); software used to prepare material for publication: SHELXL97.
cis-Dichlorobis[2-(2-pyridyl)-1
H-imidazole-
κN3]zinc(II)
hemihydrate
top
Crystal data top
[ZnCl2(C8H7N3)2]·0.5H2O | F(000) = 884 |
Mr = 435.62 | Dx = 1.557 Mg m−3 |
Orthorhombic, Pnna | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2a 2bc | Cell parameters from 1500 reflections |
a = 9.279 (5) Å | θ = 2.1–28.3° |
b = 16.055 (5) Å | µ = 1.62 mm−1 |
c = 12.474 (5) Å | T = 293 K |
V = 1858.3 (14) Å3 | Block, colorless |
Z = 4 | 0.32 × 0.29 × 0.28 mm |
Data collection top
Bruker APEX CCD area-detector diffractometer | 2222 independent reflections |
Radiation source: fine-focus sealed tube | 1740 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.049 |
φ and ω scans | θmax = 28.3°, θmin = 2.1° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −9→12 |
Tmin = 0.210, Tmax = 0.218 | k = −21→13 |
10539 measured reflections | l = −15→16 |
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)] = 0.028 | H atoms treated by a mixture of independent and constrained refinement |
wR(F2) = 0.091 | w = 1/[σ2(Fo2) + (0.0581P)2] where P = (Fo2 + 2Fc2)/3 |
S = 1.05 | (Δ/σ)max = 0.001 |
2222 reflections | Δρmax = 0.40 e Å−3 |
130 parameters | Δρmin = −0.18 e Å−3 |
3 restraints | Extinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
Primary atom site location: structure-invariant direct methods | Extinction coefficient: 0.0031 (6) |
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 | x | y | z | Uiso*/Ueq | Occ. (<1) |
C1 | 0.6967 (2) | 0.10776 (12) | 0.27670 (17) | 0.0531 (5) | |
H1 | 0.7205 | 0.1076 | 0.3491 | 0.064* | |
C2 | 0.5880 (3) | 0.05656 (15) | 0.24238 (16) | 0.0616 (6) | |
H2 | 0.5399 | 0.0220 | 0.2903 | 0.074* | |
C3 | 0.5513 (2) | 0.05737 (13) | 0.13530 (19) | 0.0685 (6) | |
H3 | 0.4762 | 0.0243 | 0.1104 | 0.082* | |
C4 | 0.6268 (2) | 0.10759 (11) | 0.06517 (17) | 0.0590 (5) | |
H4 | 0.6056 | 0.1078 | −0.0077 | 0.071* | |
C5 | 0.73536 (17) | 0.15782 (10) | 0.10670 (14) | 0.0430 (4) | |
C6 | 0.82012 (18) | 0.21589 (11) | 0.04298 (13) | 0.0420 (4) | |
C7 | 0.9724 (2) | 0.31290 (13) | 0.00626 (15) | 0.0533 (5) | |
H7 | 1.0438 | 0.3531 | 0.0136 | 0.064* | |
C8 | 0.9047 (2) | 0.29267 (14) | −0.08702 (15) | 0.0593 (5) | |
H8 | 0.9205 | 0.3162 | −0.1541 | 0.071* | |
N1 | 0.91890 (17) | 0.26482 (9) | 0.08722 (13) | 0.0430 (4) | |
N2 | 0.80971 (18) | 0.23158 (11) | −0.06266 (13) | 0.0525 (4) | |
N3 | 0.77016 (15) | 0.15796 (9) | 0.21100 (12) | 0.0431 (3) | |
Cl1 | 1.12895 (5) | 0.36368 (3) | 0.26218 (3) | 0.04627 (15) | |
Zn1 | 0.95416 (3) | 0.2500 | 0.2500 | 0.04107 (14) | |
O1W | 0.2500 | 0.5000 | 0.0704 (4) | 0.1045 (17) | 0.50 |
H5 | 0.752 (2) | 0.2060 (14) | −0.1113 (16) | 0.068 (6)* | |
H1A | 0.178 (8) | 0.492 (6) | 0.031 (7) | 0.102* | 0.25 |
H1B | 0.257 (10) | 0.457 (4) | 0.109 (7) | 0.102* | 0.25 |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
C1 | 0.0581 (12) | 0.0482 (10) | 0.0530 (10) | −0.0007 (9) | 0.0088 (9) | 0.0032 (9) |
C2 | 0.0619 (13) | 0.0469 (12) | 0.0759 (16) | −0.0093 (10) | 0.0139 (10) | 0.0040 (9) |
C3 | 0.0652 (14) | 0.0562 (12) | 0.0842 (16) | −0.0181 (10) | −0.0028 (11) | −0.0016 (12) |
C4 | 0.0605 (12) | 0.0550 (11) | 0.0614 (13) | −0.0126 (10) | −0.0107 (9) | −0.0025 (10) |
C5 | 0.0402 (9) | 0.0400 (9) | 0.0488 (9) | 0.0019 (7) | −0.0022 (7) | −0.0016 (7) |
C6 | 0.0412 (9) | 0.0446 (9) | 0.0403 (9) | 0.0014 (8) | −0.0067 (7) | −0.0025 (8) |
C7 | 0.0521 (11) | 0.0610 (12) | 0.0469 (10) | −0.0120 (9) | −0.0055 (8) | 0.0099 (9) |
C8 | 0.0584 (11) | 0.0762 (14) | 0.0431 (10) | −0.0123 (11) | −0.0070 (9) | 0.0149 (10) |
N1 | 0.0435 (8) | 0.0486 (8) | 0.0368 (8) | −0.0049 (6) | −0.0039 (7) | 0.0026 (6) |
N2 | 0.0496 (9) | 0.0666 (10) | 0.0413 (9) | −0.0077 (7) | −0.0107 (7) | 0.0013 (8) |
N3 | 0.0430 (8) | 0.0424 (8) | 0.0438 (7) | −0.0004 (6) | 0.0024 (6) | −0.0010 (7) |
Cl1 | 0.0479 (3) | 0.0454 (3) | 0.0455 (3) | −0.00158 (18) | −0.00588 (17) | −0.00051 (17) |
Zn1 | 0.0431 (2) | 0.0483 (2) | 0.03185 (19) | 0.000 | 0.000 | −0.00009 (11) |
O1W | 0.144 (6) | 0.080 (3) | 0.089 (4) | 0.019 (3) | 0.000 | 0.000 |
Geometric parameters (Å, º) top
C1—N3 | 1.336 (2) | C7—N1 | 1.365 (2) |
C1—C2 | 1.370 (3) | C7—H7 | 0.9300 |
C1—H1 | 0.9300 | C8—N2 | 1.353 (3) |
C2—C3 | 1.378 (3) | C8—H8 | 0.9300 |
C2—H2 | 0.9300 | N1—Zn1 | 2.0704 (18) |
C3—C4 | 1.380 (3) | N2—H5 | 0.91 (2) |
C3—H3 | 0.9300 | N3—Zn1 | 2.3099 (16) |
C4—C5 | 1.391 (2) | Cl1—Zn1 | 2.4463 (9) |
C4—H4 | 0.9300 | Zn1—N1i | 2.0704 (18) |
C5—N3 | 1.340 (2) | Zn1—N3i | 2.3099 (16) |
C5—C6 | 1.456 (2) | Zn1—Cl1i | 2.4463 (9) |
C6—N1 | 1.327 (2) | O1W—H1A | 0.841 (10) |
C6—N2 | 1.345 (2) | O1W—H1B | 0.842 (10) |
C7—C8 | 1.362 (3) | | |
| | | |
N3—C1—C2 | 123.08 (19) | C6—N1—Zn1 | 116.68 (12) |
N3—C1—H1 | 118.5 | C7—N1—Zn1 | 137.16 (13) |
C2—C1—H1 | 118.5 | C6—N2—C8 | 108.00 (16) |
C1—C2—C3 | 118.6 (2) | C6—N2—H5 | 127.7 (13) |
C1—C2—H2 | 120.7 | C8—N2—H5 | 124.2 (13) |
C3—C2—H2 | 120.7 | C1—N3—C5 | 118.12 (16) |
C2—C3—C4 | 119.6 (2) | C1—N3—Zn1 | 129.32 (13) |
C2—C3—H3 | 120.2 | C5—N3—Zn1 | 112.55 (11) |
C4—C3—H3 | 120.2 | N1i—Zn1—N1 | 161.81 (9) |
C3—C4—C5 | 118.04 (19) | N1i—Zn1—N3 | 90.93 (6) |
C3—C4—H4 | 121.0 | N1—Zn1—N3 | 75.53 (6) |
C5—C4—H4 | 121.0 | N1i—Zn1—N3i | 75.53 (6) |
N3—C5—C4 | 122.49 (16) | N1—Zn1—N3i | 90.93 (6) |
N3—C5—C6 | 113.50 (15) | N3—Zn1—N3i | 84.68 (8) |
C4—C5—C6 | 124.01 (16) | N1i—Zn1—Cl1 | 97.45 (4) |
N1—C6—N2 | 110.25 (17) | N1—Zn1—Cl1 | 94.59 (4) |
N1—C6—C5 | 121.67 (15) | N3—Zn1—Cl1 | 168.64 (4) |
N2—C6—C5 | 128.03 (16) | N3i—Zn1—Cl1 | 89.98 (5) |
C8—C7—N1 | 109.24 (17) | N1i—Zn1—Cl1i | 94.59 (4) |
C8—C7—H7 | 125.4 | N1—Zn1—Cl1i | 97.45 (4) |
N1—C7—H7 | 125.4 | N3—Zn1—Cl1i | 89.98 (5) |
N2—C8—C7 | 106.35 (16) | N3i—Zn1—Cl1i | 168.64 (4) |
N2—C8—H8 | 126.8 | Cl1—Zn1—Cl1i | 96.95 (4) |
C7—C8—H8 | 126.8 | H1A—O1W—H1B | 105.7 (17) |
C6—N1—C7 | 106.16 (15) | | |
| | | |
N3—C1—C2—C3 | −0.7 (3) | C6—C5—N3—C1 | 178.86 (15) |
C1—C2—C3—C4 | 1.7 (3) | C4—C5—N3—Zn1 | −179.55 (14) |
C2—C3—C4—C5 | −1.9 (3) | C6—C5—N3—Zn1 | −0.56 (17) |
C3—C4—C5—N3 | 1.1 (3) | C7—N1—Zn1—N1i | 135.6 (2) |
C3—C4—C5—C6 | −177.77 (17) | C6—N1—Zn1—N3 | −2.43 (13) |
N3—C5—C6—N1 | −1.6 (2) | C7—N1—Zn1—N3 | 178.6 (2) |
C4—C5—C6—N1 | 177.36 (18) | C6—N1—Zn1—N3i | −86.69 (14) |
N3—C5—C6—N2 | −178.63 (17) | C7—N1—Zn1—N3i | 94.3 (2) |
C4—C5—C6—N2 | 0.3 (3) | C6—N1—Zn1—Cl1 | −176.75 (13) |
N1—C7—C8—N2 | −0.3 (2) | C7—N1—Zn1—Cl1 | 4.2 (2) |
N2—C6—N1—C7 | 0.0 (2) | C6—N1—Zn1—Cl1i | 85.62 (13) |
C5—C6—N1—C7 | −177.53 (16) | C7—N1—Zn1—Cl1i | −93.4 (2) |
N2—C6—N1—Zn1 | −179.33 (12) | C1—N3—Zn1—N1i | −10.03 (15) |
C5—C6—N1—Zn1 | 3.2 (2) | C5—N3—Zn1—N1i | 169.30 (12) |
C8—C7—N1—C6 | 0.2 (2) | C1—N3—Zn1—N1 | −177.75 (16) |
C8—C7—N1—Zn1 | 179.26 (15) | C5—N3—Zn1—N1 | 1.59 (11) |
N1—C6—N2—C8 | −0.1 (2) | C1—N3—Zn1—N3i | −85.41 (15) |
C5—C6—N2—C8 | 177.17 (18) | C5—N3—Zn1—N3i | 93.93 (12) |
C7—C8—N2—C6 | 0.2 (2) | C1—N3—Zn1—Cl1 | −147.68 (16) |
C2—C1—N3—C5 | −0.1 (3) | C5—N3—Zn1—Cl1 | 31.7 (3) |
C2—C1—N3—Zn1 | 179.23 (16) | C1—N3—Zn1—Cl1i | 84.55 (15) |
C4—C5—N3—C1 | −0.1 (3) | C5—N3—Zn1—Cl1i | −96.11 (11) |
Symmetry code: (i) 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 |
N2—H5···Cl1ii | 0.91 (2) | 2.25 (2) | 3.151 (2) | 174.3 (18) |
Symmetry code: (ii) x−1/2, −y+1/2, z−1/2. |