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The title compound, (C6H10N2)[ZnI4]·2H2O, crystallizes as an organic–inorganic hybrid. The ionic layer consists of isolated ZnI4 tetrahedra. The hydrocarbon layer has two symmetry-independant centrosymmetric p-phenylenediammonium cations that link to the ionic layer via hydrogen bonding. Two water molecules of hydration lie between the anion and the two cations.
Supporting information
CCDC reference: 604985
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (C-C) = 0.008 Å
- R factor = 0.027
- wR factor = 0.071
- Data-to-parameter ratio = 24.1
checkCIF/PLATON results
No syntax errors found
Alert level B
PLAT417_ALERT_2_B Short Inter D-H..H-D H1B .. H12 .. 1.88 Ang.
PLAT417_ALERT_2_B Short Inter D-H..H-D H1C .. H11 .. 1.81 Ang.
PLAT420_ALERT_2_B D-H Without Acceptor O1 - H11 ... ?
PLAT420_ALERT_2_B D-H Without Acceptor O1 - H12 ... ?
Alert level C
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ?
PLAT199_ALERT_1_C Check the Reported _cell_measurement_temperature 293 K
PLAT420_ALERT_2_C D-H Without Acceptor N2 - H2A ... ?
PLAT480_ALERT_4_C Long H...A H-Bond Reported H2A .. I3 .. 3.14 Ang.
PLAT480_ALERT_4_C Long H...A H-Bond Reported H2A .. I3 .. 3.19 Ang.
PLAT480_ALERT_4_C Long H...A H-Bond Reported H2C .. I4 .. 3.21 Ang.
PLAT480_ALERT_4_C Long H...A H-Bond Reported H12 .. I4 .. 3.07 Ang.
PLAT480_ALERT_4_C Long H...A H-Bond Reported H11 .. I3 .. 3.18 Ang.
PLAT481_ALERT_4_C Long D...A H-Bond Reported O1 .. I3 .. 4.03 Ang.
PLAT764_ALERT_4_C Overcomplete CIF Bond List Detected (Rep/Expd) . 1.17 Ratio
0 ALERT level A = In general: serious problem
4 ALERT level B = Potentially serious problem
10 ALERT level C = Check and explain
0 ALERT level G = General alerts; check
2 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
5 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
7 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: SMART-NT (Bruker, 1998); cell refinement: SAINT-Plus (Bruker, 1999); data reduction: XPREP (Bruker, 1999); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997) and DIAMOND (Brandenburg, 1999); software used to prepare material for publication: WinGX (Farrugia, 1999) and PLATON (Spek, 2002).
p-Phenylenediammonium tetraiodozincate(II) dihydrate
top
Crystal data top
(C6H10N2)[ZnI4]·2H2O | Z = 2 |
Mr = 719.16 | F(000) = 644 |
Triclinic, P1 | Dx = 2.787 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71069 Å |
a = 8.398 (5) Å | Cell parameters from 927 reflections |
b = 8.611 (5) Å | θ = 2.6–28.2° |
c = 12.540 (5) Å | µ = 8.63 mm−1 |
α = 92.821 (5)° | T = 293 K |
β = 103.344 (5)° | Plate, colourless |
γ = 102.407 (5)° | 0.35 × 0.20 × 0.08 mm |
V = 857.1 (8) Å3 | |
Data collection top
Bruker SMART CCD area-detector diffractometer | 2967 reflections with I > 2σ(I) |
φ and ω scans | Rint = 0.034 |
Absorption correction: integration (XPREP; Bruker, 1999) | θmax = 26°, θmin = 1.7° |
Tmin = 0.152, Tmax = 0.545 | h = −9→10 |
5108 measured reflections | k = −10→7 |
3352 independent reflections | l = −15→15 |
Refinement top
Refinement on F2 | H-atom parameters constrained |
Least-squares matrix: full | w = 1/[σ2(Fo2) + (0.0333P)2 + 1.4644P] where P = (Fo2 + 2Fc2)/3 |
R[F2 > 2σ(F2)] = 0.028 | (Δ/σ)max < 0.001 |
wR(F2) = 0.071 | Δρmax = 1.01 e Å−3 |
S = 1.08 | Δρmin = −0.65 e Å−3 |
3352 reflections | Extinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
139 parameters | Extinction coefficient: 0.0036 (3) |
2 restraints | |
Special details top
Experimental. Numerical integration absroption corrections based on indexed crystal faces were
applied using the XPREP routine (Bruker, 1999) |
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. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
C1' | 0.1066 (6) | 0.1451 (6) | 0.5283 (4) | 0.0363 (11) | |
C1 | 0.6584 (6) | 0.0788 (6) | 1.0000 (4) | 0.0375 (11) | |
C2' | −0.0573 (7) | 0.1270 (6) | 0.5353 (5) | 0.0442 (13) | |
H2' | −0.094 | 0.2137 | 0.5595 | 0.053* | |
C2 | 0.5760 (7) | 0.1419 (7) | 1.0678 (5) | 0.0471 (13) | |
H2 | 0.6276 | 0.2366 | 1.113 | 0.057* | |
C3' | 0.1663 (7) | 0.0210 (7) | 0.4941 (5) | 0.0435 (12) | |
H3' | 0.278 | 0.0361 | 0.4908 | 0.052* | |
C3 | 0.5864 (7) | −0.0610 (6) | 0.9326 (5) | 0.0443 (13) | |
H3 | 0.6454 | −0.1013 | 0.8878 | 0.053* | |
N1 | 0.8301 (6) | 0.1622 (6) | 1.0000 (4) | 0.0480 (11) | |
H1A | 0.8368 | 0.2669 | 1.0013 | 0.072* | |
H1B | 0.8559 | 0.1275 | 0.9396 | 0.072* | |
H1C | 0.9019 | 0.1429 | 1.0593 | 0.072* | |
N2 | 0.2201 (6) | 0.3042 (5) | 0.5602 (4) | 0.0426 (10) | |
H2A | 0.1609 | 0.3786 | 0.5476 | 0.064* | |
H2B | 0.2967 | 0.3171 | 0.5209 | 0.064* | |
H2C | 0.2712 | 0.3135 | 0.6316 | 0.064* | |
Zn1 | 0.26937 (8) | 0.49774 (7) | 0.25256 (5) | 0.03962 (16) | |
I1 | 0.46803 (5) | 0.32644 (4) | 0.35242 (3) | 0.04260 (12) | |
I2 | 0.23975 (5) | 0.44197 (5) | 0.04017 (3) | 0.04666 (12) | |
I3 | −0.02339 (5) | 0.41033 (5) | 0.29980 (3) | 0.04676 (12) | |
I4 | 0.38434 (5) | 0.80474 (4) | 0.30372 (3) | 0.04486 (12) | |
O1 | 0.0187 (6) | 0.9959 (6) | 0.1569 (4) | 0.0681 (13) | |
H11 | 0.0094 | 1.083 | 0.187 | 0.082* | |
H12 | 0.0976 | 0.9541 | 0.1886 | 0.082* | |
O2 | 0.7494 (8) | 0.7684 (8) | 0.2082 (4) | 0.0936 (19) | |
H21 | 0.7382 | 0.6932 | 0.159 | 0.112* | |
H22 | 0.6673 | 0.8137 | 0.1964 | 0.112* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
C1' | 0.037 (3) | 0.036 (3) | 0.033 (2) | 0.000 (2) | 0.011 (2) | 0.000 (2) |
C1 | 0.037 (3) | 0.034 (3) | 0.041 (3) | 0.007 (2) | 0.008 (2) | 0.012 (2) |
C2' | 0.040 (3) | 0.036 (3) | 0.059 (3) | 0.005 (2) | 0.021 (3) | −0.002 (2) |
C2 | 0.049 (3) | 0.037 (3) | 0.052 (3) | −0.001 (2) | 0.018 (3) | −0.002 (2) |
C3' | 0.033 (3) | 0.045 (3) | 0.053 (3) | 0.004 (2) | 0.016 (2) | 0.004 (2) |
C3 | 0.050 (3) | 0.036 (3) | 0.053 (3) | 0.009 (2) | 0.025 (3) | 0.001 (2) |
N1 | 0.039 (3) | 0.044 (3) | 0.061 (3) | 0.005 (2) | 0.016 (2) | 0.010 (2) |
N2 | 0.041 (2) | 0.033 (2) | 0.049 (3) | −0.0013 (19) | 0.013 (2) | 0.0008 (19) |
Zn1 | 0.0408 (3) | 0.0376 (3) | 0.0407 (3) | 0.0062 (3) | 0.0128 (3) | 0.0053 (3) |
I1 | 0.0467 (2) | 0.03722 (19) | 0.0458 (2) | 0.01165 (15) | 0.01293 (16) | 0.00718 (14) |
I2 | 0.0562 (2) | 0.0495 (2) | 0.0383 (2) | 0.01547 (17) | 0.01656 (16) | 0.00482 (15) |
I3 | 0.0385 (2) | 0.0532 (2) | 0.0490 (2) | 0.00593 (16) | 0.01617 (16) | 0.00456 (16) |
I4 | 0.0492 (2) | 0.03392 (19) | 0.0504 (2) | 0.00781 (15) | 0.01211 (16) | 0.00406 (15) |
O1 | 0.067 (3) | 0.083 (3) | 0.060 (3) | 0.031 (3) | 0.013 (2) | 0.013 (2) |
O2 | 0.102 (4) | 0.125 (5) | 0.059 (3) | 0.027 (4) | 0.033 (3) | −0.011 (3) |
Geometric parameters (Å, º) top
C1'—C3' | 1.363 (7) | N1—H1A | 0.89 |
C1'—C2' | 1.376 (7) | N1—H1B | 0.89 |
C1'—N2 | 1.468 (6) | N1—H1C | 0.89 |
C1—C3 | 1.371 (7) | N2—H2A | 0.89 |
C1—C2 | 1.373 (8) | N2—H2B | 0.89 |
C1—N1 | 1.466 (7) | N2—H2C | 0.89 |
C2'—C3'i | 1.377 (7) | Zn1—I4 | 2.6043 (16) |
C2'—H2' | 0.93 | Zn1—I1 | 2.6081 (12) |
C2—C3ii | 1.390 (8) | Zn1—I3 | 2.6236 (15) |
C2—H2 | 0.93 | Zn1—I2 | 2.6274 (13) |
C3'—C2'i | 1.377 (7) | O1—H11 | 0.8502 |
C3'—H3' | 0.93 | O1—H12 | 0.8496 |
C3—C2ii | 1.390 (8) | O2—H21 | 0.8461 |
C3—H3 | 0.93 | O2—H22 | 0.851 |
| | | |
C3'—C1'—C2' | 122.4 (5) | C1—N1—H1B | 109.5 |
C3'—C1'—N2 | 119.6 (5) | H1A—N1—H1B | 109.5 |
C2'—C1'—N2 | 118.0 (5) | C1—N1—H1C | 109.5 |
C3—C1—C2 | 122.3 (5) | H1A—N1—H1C | 109.5 |
C3—C1—N1 | 118.5 (5) | H1B—N1—H1C | 109.5 |
C2—C1—N1 | 119.2 (5) | C1'—N2—H2A | 109.5 |
C1'—C2'—C3'i | 119.1 (5) | C1'—N2—H2B | 109.5 |
C1'—C2'—H2' | 120.4 | H2A—N2—H2B | 109.5 |
C3'i—C2'—H2' | 120.4 | C1'—N2—H2C | 109.5 |
C1—C2—C3ii | 118.6 (5) | H2A—N2—H2C | 109.5 |
C1—C2—H2 | 120.7 | H2B—N2—H2C | 109.5 |
C3ii—C2—H2 | 120.7 | I4—Zn1—I1 | 114.06 (4) |
C1'—C3'—C2'i | 118.4 (5) | I4—Zn1—I3 | 109.25 (3) |
C1'—C3'—H3' | 120.8 | I1—Zn1—I3 | 108.64 (4) |
C2'i—C3'—H3' | 120.8 | I4—Zn1—I2 | 106.87 (3) |
C1—C3—C2ii | 119.1 (5) | I1—Zn1—I2 | 107.10 (3) |
C1—C3—H3 | 120.4 | I3—Zn1—I2 | 110.91 (3) |
C2ii—C3—H3 | 120.4 | H11—O1—H12 | 118.3 |
C1—N1—H1A | 109.5 | H21—O2—H22 | 112.8 |
| | | |
C3'—C1'—C2'—C3'i | −0.6 (10) | C2'—C1'—C3'—C2'i | 0.6 (10) |
N2—C1'—C2'—C3'i | −180.0 (5) | N2—C1'—C3'—C2'i | 180.0 (5) |
C3—C1—C2—C3ii | −0.4 (10) | C2—C1—C3—C2ii | 0.4 (10) |
N1—C1—C2—C3ii | −179.6 (5) | N1—C1—C3—C2ii | 179.6 (5) |
Symmetry codes: (i) −x, −y, −z+1; (ii) −x+1, −y, −z+2. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
N1—H1A···I2iii | 0.89 | 2.76 | 3.620 (5) | 162 |
N1—H1B···O1iii | 0.89 | 2.16 | 2.995 (7) | 157 |
N1—H1C···O1iv | 0.89 | 2.05 | 2.871 (7) | 153 |
N2—H2A···I3v | 0.89 | 3.14 | 3.809 (5) | 133 |
N2—H2A···I3 | 0.89 | 3.19 | 3.701 (5) | 119 |
N2—H2B···I1 | 0.89 | 2.81 | 3.681 (5) | 166 |
N2—H2C···O2iii | 0.89 | 2.19 | 2.966 (7) | 145 |
N2—H2C···I4iii | 0.89 | 3.21 | 3.703 (5) | 117 |
O1—H12···I4 | 0.85 | 3.07 | 3.923 (5) | 180 |
O1—H11···I3vi | 0.85 | 3.18 | 4.034 (6) | 180 |
O2—H21···I2vii | 0.85 | 2.77 | 3.554 (5) | 156 |
O2—H22···I4 | 0.85 | 2.98 | 3.606 (6) | 132 |
Symmetry codes: (iii) −x+1, −y+1, −z+1; (iv) x+1, y−1, z+1; (v) −x, −y+1, −z+1; (vi) x, y+1, z; (vii) −x+1, −y+1, −z. |
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