Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536803012674/tk6114sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536803012674/tk6114Isup2.hkl |
CCDC reference: 196405
The reaction of zinc dipicrate octahydrate with 4,4'-bipyridine gives bis(4,4'-bipyridine)diaquazinc dipicrate (Liang et al., 2000) as a dihydrate (Liang et al., 2001b) as well as a monohydrated co-crystal with 4,4'-bipyridine (Liang et al., 2001a).
The aromatic H atoms were generated geometrically (C—H = 0.93 Å) in a riding-model approximation, and were assigned displacement parameters 1.2 times those of their parent C atoms. The water H atoms were located and refined, subject to O—H = 0.85±0.01 Å and H···H = 1.39±0.01 Å; the displacement parameters were similarly assigned. The aromatic ring of the anion was refined as a rigid hexagon (C—C = 1.39 Å); the three C—N distances were restrained to be approximately equal within ±0.01 Å as were the six N—O distances.
Data collection: CAD-4 Software (Enraf-Nonius, 1988); cell refinement: CAD-4 Software; data reduction: XCAD4 (Harms, 1997); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEPII (Johnson, 1976); software used to prepare material for publication: SHELXL97.
Fig. 1. ORTEPII (Johnson, 1976) plot of a portion of the crystal structure of (I), with ellipsoids drawn at the 50% probability level. |
[Zn(C10H8N2)2(H2O)2](C6H2N3O7)2·2H2O | F(000) = 1856 |
Mr = 906.01 | Dx = 1.605 Mg m−3 |
Monoclinic, C2/c | Mo Kα radiation, λ = 0.71073 Å |
a = 14.391 (2) Å | Cell parameters from 25 reflections |
b = 11.418 (1) Å | θ = 15.4–15.9° |
c = 22.908 (3) Å | µ = 0.75 mm−1 |
β = 95.08 (1)° | T = 298 K |
V = 3749.4 (8) Å3 | Block, yellow |
Z = 4 | 0.18 × 0.15 × 0.12 mm |
Enraf-Nonius CAD-4 diffractometer | 2020 reflections with I > 2σ(I) |
Radiation source: fine-focus sealed tube | Rint = 0.021 |
Graphite monochromator | θmax = 26.0°, θmin = 1.8° |
ω scans | h = −17→0 |
Absorption correction: empirical VIA ψ scan (North et al., 1968) | k = −14→0 |
Tmin = 0.874, Tmax = 0.914 | l = −28→28 |
3829 measured reflections | 2 standard reflections every 60 min |
3679 independent reflections | intensity decay: none |
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)] = 0.057 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.152 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.01 | w = 1/[σ2(Fo2) + (0.0526P)2 + 9.5165P] where P = (Fo2 + 2Fc2)/3 |
3679 reflections | (Δ/σ)max = 0.001 |
278 parameters | Δρmax = 0.61 e Å−3 |
24 restraints | Δρmin = −0.60 e Å−3 |
[Zn(C10H8N2)2(H2O)2](C6H2N3O7)2·2H2O | V = 3749.4 (8) Å3 |
Mr = 906.01 | Z = 4 |
Monoclinic, C2/c | Mo Kα radiation |
a = 14.391 (2) Å | µ = 0.75 mm−1 |
b = 11.418 (1) Å | T = 298 K |
c = 22.908 (3) Å | 0.18 × 0.15 × 0.12 mm |
β = 95.08 (1)° |
Enraf-Nonius CAD-4 diffractometer | 2020 reflections with I > 2σ(I) |
Absorption correction: empirical VIA ψ scan (North et al., 1968) | Rint = 0.021 |
Tmin = 0.874, Tmax = 0.914 | 2 standard reflections every 60 min |
3829 measured reflections | intensity decay: none |
3679 independent reflections |
R[F2 > 2σ(F2)] = 0.057 | 24 restraints |
wR(F2) = 0.152 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.01 | Δρmax = 0.61 e Å−3 |
3679 reflections | Δρmin = −0.60 e Å−3 |
278 parameters |
x | y | z | Uiso*/Ueq | ||
Zn1 | 0.5000 | 0.49511 (8) | 0.2500 | 0.0309 (2) | |
O1 | 0.2599 (3) | 0.4267 (4) | 0.1471 (2) | 0.068 (1) | |
O2 | 0.2301 (5) | 0.6563 (5) | 0.1555 (2) | 0.113 (2) | |
O3 | 0.2327 (5) | 0.7448 (5) | 0.0736 (3) | 0.113 (2) | |
O4 | 0.0503 (5) | 0.5755 (7) | −0.0891 (2) | 0.120 (3) | |
O5 | 0.0286 (4) | 0.3882 (7) | −0.0935 (2) | 0.122 (3) | |
O6 | 0.1809 (4) | 0.1412 (5) | 0.0504 (3) | 0.109 (2) | |
O7 | 0.2297 (7) | 0.2052 (6) | 0.1321 (3) | 0.178 (4) | |
O1w | 0.3524 (2) | 0.4994 (4) | 0.2481 (1) | 0.041 (1) | |
O2w | 0.2530 (4) | 0.4529 (4) | 0.3416 (1) | 0.069 (1) | |
N1 | 0.5000 | 0.6852 (5) | 0.2500 | 0.036 (2) | |
N2 | 0.5000 | 1.3048 (5) | 0.2500 | 0.031 (1) | |
N3 | 0.5084 (3) | 0.4938 (4) | 0.3458 (1) | 0.035 (1) | |
N4 | 0.2217 (4) | 0.6580 (5) | 0.1025 (2) | 0.073 (2) | |
N5 | 0.0620 (4) | 0.4765 (7) | −0.0697 (2) | 0.095 (3) | |
N6 | 0.1970 (5) | 0.2217 (5) | 0.0832 (3) | 0.078 (2) | |
C1 | 0.5733 (4) | 0.7474 (4) | 0.2359 (2) | 0.044 (1) | |
C2 | 0.5758 (4) | 0.8676 (5) | 0.2356 (2) | 0.044 (1) | |
C3 | 0.5000 | 0.9309 (6) | 0.2500 | 0.035 (2) | |
C4 | 0.5000 | 1.0593 (7) | 0.2500 | 0.038 (2) | |
C5 | 0.5786 (4) | 1.1226 (4) | 0.2704 (2) | 0.044 (1) | |
C6 | 0.5750 (4) | 1.2431 (4) | 0.2700 (2) | 0.039 (1) | |
C7 | 0.4739 (4) | 0.4060 (5) | 0.3745 (2) | 0.046 (1) | |
C8 | 0.4699 (4) | 0.4055 (5) | 0.4343 (2) | 0.045 (1) | |
C9 | 0.5036 (3) | 0.4981 (5) | 0.4679 (2) | 0.035 (1) | |
C10 | 0.5424 (4) | 0.5872 (5) | 0.4379 (2) | 0.056 (2) | |
C11 | 0.5426 (4) | 0.5826 (5) | 0.3781 (2) | 0.051 (2) | |
C12 | 0.2131 (3) | 0.4392 (4) | 0.0960 (1) | 0.053 (2) | |
C13 | 0.1966 (3) | 0.5501 (3) | 0.0723 (2) | 0.059 (2) | |
C14 | 0.1482 (3) | 0.5625 (3) | 0.0174 (2) | 0.063 (2) | |
C15 | 0.1163 (2) | 0.4639 (4) | −0.0138 (1) | 0.062 (2) | |
C16 | 0.1327 (3) | 0.3530 (3) | 0.0099 (2) | 0.061 (2) | |
C17 | 0.1811 (3) | 0.3406 (3) | 0.0648 (2) | 0.050 (2) | |
H1w1 | 0.321 (3) | 0.476 (4) | 0.275 (1) | 0.049* | |
H1w2 | 0.322 (3) | 0.487 (5) | 0.215 (1) | 0.049* | |
H2w1 | 0.253 (5) | 0.383 (2) | 0.355 (2) | 0.083* | |
H2w2 | 0.263 (5) | 0.500 (3) | 0.370 (2) | 0.083* | |
H1 | 0.6255 | 0.7070 | 0.2256 | 0.052* | |
H2 | 0.6290 | 0.9062 | 0.2256 | 0.053* | |
H5 | 0.6331 | 1.0840 | 0.2842 | 0.053* | |
H6 | 0.6279 | 1.2840 | 0.2845 | 0.047* | |
H7 | 0.4512 | 0.3412 | 0.3532 | 0.055* | |
H8 | 0.4440 | 0.3416 | 0.4522 | 0.054* | |
H10 | 0.5688 | 0.6512 | 0.4583 | 0.067* | |
H11 | 0.5683 | 0.6454 | 0.3592 | 0.062* | |
H14 | 0.1373 | 0.6367 | 0.0016 | 0.076* | |
H16 | 0.1113 | 0.2870 | −0.0110 | 0.073* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Zn1 | 0.0414 (5) | 0.0269 (4) | 0.0241 (4) | 0.000 | 0.0007 (3) | 0.000 |
O1 | 0.074 (3) | 0.066 (3) | 0.059 (3) | −0.004 (3) | −0.015 (2) | −0.002 (2) |
O2 | 0.176 (6) | 0.083 (4) | 0.076 (4) | 0.018 (4) | −0.022 (4) | −0.034 (3) |
O3 | 0.160 (6) | 0.057 (3) | 0.124 (5) | 0.006 (4) | 0.019 (4) | 0.005 (4) |
O4 | 0.100 (5) | 0.198 (8) | 0.059 (4) | 0.038 (5) | −0.005 (3) | 0.032 (4) |
O5 | 0.097 (5) | 0.207 (8) | 0.057 (4) | 0.010 (5) | −0.018 (3) | −0.034 (4) |
O6 | 0.114 (5) | 0.075 (4) | 0.137 (5) | −0.022 (4) | 0.010 (4) | −0.022 (4) |
O7 | 0.30 (1) | 0.076 (5) | 0.142 (6) | 0.002 (6) | −0.088 (7) | 0.021 (5) |
O1w | 0.042 (2) | 0.045 (2) | 0.036 (2) | −0.006 (2) | 0.001 (1) | −0.001 (2) |
O2w | 0.071 (3) | 0.072 (3) | 0.064 (3) | 0.006 (3) | 0.010 (3) | 0.013 (2) |
N1 | 0.047 (4) | 0.027 (3) | 0.036 (4) | 0.000 | 0.008 (3) | 0.000 |
N2 | 0.042 (4) | 0.029 (3) | 0.022 (3) | 0.000 | −0.004 (3) | 0.000 |
N3 | 0.039 (2) | 0.039 (2) | 0.025 (2) | −0.004 (3) | −0.000 (2) | 0.001 (2) |
N4 | 0.080 (4) | 0.063 (4) | 0.074 (4) | 0.017 (4) | −0.002 (3) | −0.015 (4) |
N5 | 0.065 (4) | 0.172 (9) | 0.046 (4) | 0.021 (5) | −0.002 (3) | −0.002 (5) |
N6 | 0.079 (5) | 0.066 (4) | 0.088 (5) | 0.002 (4) | 0.006 (4) | −0.004 (4) |
C1 | 0.049 (4) | 0.027 (3) | 0.057 (4) | 0.008 (3) | 0.019 (3) | 0.001 (3) |
C2 | 0.038 (3) | 0.031 (3) | 0.063 (4) | −0.002 (3) | 0.010 (3) | 0.003 (3) |
C3 | 0.044 (5) | 0.029 (4) | 0.030 (4) | 0.000 | −0.005 (4) | 0.000 |
C4 | 0.051 (6) | 0.026 (4) | 0.038 (5) | 0.000 | 0.006 (4) | 0.000 |
C5 | 0.048 (4) | 0.029 (3) | 0.054 (3) | 0.003 (3) | −0.009 (3) | 0.003 (3) |
C6 | 0.042 (3) | 0.030 (3) | 0.043 (3) | 0.000 (2) | −0.009 (2) | 0.002 (2) |
C7 | 0.075 (4) | 0.038 (3) | 0.024 (3) | −0.007 (3) | 0.001 (3) | −0.002 (2) |
C8 | 0.066 (4) | 0.039 (3) | 0.030 (3) | −0.015 (3) | 0.004 (3) | −0.001 (2) |
C9 | 0.037 (3) | 0.043 (3) | 0.025 (2) | −0.002 (3) | 0.004 (2) | −0.002 (3) |
C10 | 0.077 (5) | 0.062 (4) | 0.028 (3) | −0.037 (4) | 0.004 (3) | −0.011 (3) |
C11 | 0.072 (4) | 0.053 (4) | 0.029 (3) | −0.027 (3) | 0.007 (3) | −0.001 (3) |
C12 | 0.038 (3) | 0.065 (4) | 0.054 (4) | 0.001 (3) | 0.004 (3) | 0.001 (3) |
C13 | 0.058 (4) | 0.057 (4) | 0.061 (4) | 0.006 (3) | −0.001 (3) | −0.009 (3) |
C14 | 0.054 (4) | 0.071 (5) | 0.066 (4) | 0.017 (4) | 0.017 (3) | 0.009 (4) |
C15 | 0.041 (3) | 0.103 (6) | 0.042 (3) | 0.015 (4) | 0.002 (3) | −0.006 (3) |
C16 | 0.044 (4) | 0.089 (5) | 0.051 (4) | 0.001 (4) | 0.006 (3) | −0.017 (4) |
C17 | 0.041 (3) | 0.056 (4) | 0.054 (4) | −0.007 (3) | 0.007 (3) | −0.006 (3) |
Zn1—O1w | 2.122 (3) | C4—C5i | 1.388 (6) |
Zn1—O1wi | 2.122 (3) | C5—C6 | 1.378 (7) |
Zn1—N1 | 2.170 (6) | C7—C8 | 1.377 (6) |
Zn1—N2ii | 2.173 (6) | C8—C9 | 1.370 (7) |
Zn1—N3 | 2.187 (3) | C9—C10 | 1.374 (7) |
Zn1—N3i | 2.187 (3) | C9—C9iii | 1.486 (8) |
O1—C12 | 1.306 (5) | C10—C11 | 1.370 (7) |
O2—N4 | 1.210 (5) | C12—C13 | 1.39 |
O3—N4 | 1.209 (5) | C12—C17 | 1.39 |
O4—N5 | 1.220 (6) | C13—C14 | 1.39 |
O5—N5 | 1.224 (6) | C14—C15 | 1.39 |
O6—N6 | 1.197 (5) | C15—C16 | 1.39 |
O7—N6 | 1.190 (6) | C16—C17 | 1.39 |
N1—C1i | 1.335 (6) | O1w—H1w1 | 0.85 (1) |
N1—C1 | 1.335 (6) | O1w—H1w2 | 0.85 (1) |
N2—C6i | 1.334 (6) | O2w—H2w1 | 0.85 (1) |
N2—C6 | 1.334 (6) | O2w—H2w2 | 0.85 (1) |
N3—C7 | 1.320 (6) | C1—H1 | 0.93 |
N3—C11 | 1.325 (6) | C2—H2 | 0.93 |
N4—C13 | 1.443 (5) | C5—H5 | 0.93 |
N5—C15 | 1.447 (5) | C6—H6 | 0.93 |
N6—C17 | 1.434 (6) | C7—H7 | 0.93 |
C1—C2 | 1.373 (7) | C8—H8 | 0.93 |
C2—C3 | 1.373 (6) | C10—H10 | 0.93 |
C3—C2i | 1.373 (6) | C11—H11 | 0.93 |
C3—C4 | 1.466 (9) | C14—H14 | 0.93 |
C4—C5 | 1.388 (6) | C16—H16 | 0.93 |
O1w—Zn1—O1wi | 177.4 (2) | C9—C8—C7 | 120.7 (5) |
O1w—Zn1—N1 | 88.7 (1) | C8—C9—C10 | 115.5 (4) |
O1wi—Zn1—N1 | 88.7 (1) | C8—C9—C9iii | 121.7 (6) |
O1w—Zn1—N2ii | 91.3 (1) | C10—C9—C9iii | 122.7 (6) |
O1wi—Zn1—N2ii | 91.3 (1) | C11—C10—C9 | 120.5 (5) |
N1—Zn1—N2ii | 180.0 (1) | N3—C11—C10 | 123.7 (5) |
O1w—Zn1—N3 | 89.3 (1) | O1—C12—C13 | 120.4 (4) |
O1wi—Zn1—N3 | 90.7 (1) | O1—C12—C17 | 119.6 (4) |
N1—Zn1—N3 | 90.4 (1) | C13—C12—C17 | 120 |
N2ii—Zn1—N3 | 89.6 (1) | C12—C13—C14 | 120 |
O1w—Zn1—N3i | 90.7 (1) | C12—C13—N4 | 124.4 (4) |
O1wi—Zn1—N3i | 89.3 (1) | C14—C13—N4 | 115.5 (4) |
N1—Zn1—N3i | 90.4 (1) | C13—C14—C15 | 120 |
N2ii—Zn1—N3i | 89.6 (1) | C16—C15—C14 | 120 |
N3—Zn1—N3i | 179.2 (3) | C16—C15—N5 | 119.7 (4) |
C1i—N1—C1 | 115.7 (6) | C14—C15—N5 | 120.2 (4) |
C1i—N1—Zn1 | 122.2 (3) | C15—C16—C17 | 120 |
C1—N1—Zn1 | 122.2 (3) | C16—C17—C12 | 120 |
C6i—N2—C6 | 116.4 (6) | C16—C17—N6 | 114.7 (4) |
C6i—N2—Zn1iv | 121.8 (3) | C12—C17—N6 | 125.3 (4) |
C6—N2—Zn1iv | 121.8 (3) | Zn1—O1w—H1w1 | 125 (3) |
C7—N3—C11 | 116.1 (4) | Zn1—O1w—H1w2 | 117 (3) |
C7—N3—Zn1 | 121.0 (3) | H1w1—O1w—H1w2 | 109 (2) |
C11—N3—Zn1 | 122.8 (3) | H2w1—O2w—H2w2 | 109 (2) |
O3—N4—O2 | 123.7 (6) | N1—C1—H1 | 118.1 |
O3—N4—C13 | 118.5 (6) | C2—C1—H1 | 118.1 |
O2—N4—C13 | 117.7 (6) | C1—C2—H2 | 119.9 |
O4—N5—O5 | 124.4 (7) | C3—C2—H2 | 119.9 |
O4—N5—C15 | 117.4 (6) | C6—C5—H5 | 120.4 |
O5—N5—C15 | 118.1 (6) | C4—C5—H5 | 120.4 |
O7—N6—O6 | 120.4 (7) | N2—C6—H6 | 118.0 |
O7—N6—C17 | 117.9 (6) | C5—C6—H6 | 118.0 |
O6—N6—C17 | 121.7 (6) | N3—C7—H7 | 118.3 |
N1—C1—C2 | 123.7 (5) | C8—C7—H7 | 118.3 |
C1—C2—C3 | 120.2 (6) | C9—C8—H8 | 119.6 |
C2i—C3—C2 | 116.5 (7) | C7—C8—H8 | 119.6 |
C2i—C3—C4 | 121.8 (3) | C11—C10—H10 | 119.7 |
C2—C3—C4 | 121.8 (3) | C9—C10—H10 | 119.7 |
C5—C4—C5i | 117.2 (7) | N3—C11—H11 | 118.2 |
C5—C4—C3 | 121.4 (3) | C10—C11—H11 | 118.2 |
C5i—C4—C3 | 121.4 (3) | C13—C14—H14 | 120.0 |
C6—C5—C4 | 119.3 (6) | C15—C14—H14 | 120.0 |
N2—C6—C5 | 123.9 (5) | C15—C16—H16 | 120.0 |
N3—C7—C8 | 123.4 (5) | C17—C16—H16 | 120.0 |
O1w—Zn1—N1—C1i | 17.8 (3) | C11—N3—C7—C8 | 2.1 (9) |
O1wi—Zn1—N1—C1i | −162.2 (3) | Zn1—N3—C7—C8 | −174.0 (4) |
N3—Zn1—N1—C1i | −71.5 (3) | N3—C7—C8—C9 | −0.9 (9) |
N3i—Zn1—N1—C1i | 108.5 (3) | C7—C8—C9—C10 | −1.4 (8) |
O1w—Zn1—N1—C1 | −162.2 (3) | C7—C8—C9—C9iii | 177.4 (6) |
O1wi—Zn1—N1—C1 | 17.8 (3) | C8—C9—C10—C11 | 2.5 (9) |
N3—Zn1—N1—C1 | 108.5 (3) | C9iii—C9—C10—C11 | −176.3 (6) |
N3i—Zn1—N1—C1 | −71.5 (3) | C7—N3—C11—C10 | −0.9 (9) |
O1w—Zn1—N3—C7 | 63.3 (4) | Zn1—N3—C11—C10 | 175.1 (5) |
O1wi—Zn1—N3—C7 | −119.4 (4) | C9—C10—C11—N3 | −2 (1) |
N1—Zn1—N3—C7 | 151.9 (4) | O1—C12—C13—C14 | 178.8 (4) |
N2ii—Zn1—N3—C7 | −28.1 (4) | O1—C12—C13—N4 | −5.2 (5) |
N3i—Zn1—N3—C7 | −28.1 (4) | C17—C12—C13—N4 | 176.0 (5) |
O1w—Zn1—N3—C11 | −112.6 (4) | O3—N4—C13—C12 | 156.3 (6) |
O1wi—Zn1—N3—C11 | 64.8 (4) | O2—N4—C13—C12 | −23.9 (8) |
N1—Zn1—N3—C11 | −23.9 (4) | O3—N4—C13—C14 | −27.5 (8) |
N2ii—Zn1—N3—C11 | 156.1 (4) | O2—N4—C13—C14 | 152.3 (5) |
N3i—Zn1—N3—C11 | 156.1 (4) | N4—C13—C14—C15 | −176.4 (4) |
C1i—N1—C1—C2 | 0.2 (4) | C13—C14—C15—N5 | 177.1 (4) |
Zn1—N1—C1—C2 | −179.8 (4) | O4—N5—C15—C16 | −179.2 (6) |
N1—C1—C2—C3 | −0.4 (9) | O5—N5—C15—C16 | 3.1 (8) |
C1—C2—C3—C2i | 0.2 (4) | O4—N5—C15—C14 | 3.8 (8) |
C1—C2—C3—C4 | −179.8 (4) | O5—N5—C15—C14 | −174.0 (6) |
C2i—C3—C4—C5 | 140.5 (4) | N5—C15—C16—C17 | −177.1 (4) |
C2—C3—C4—C5 | −39.5 (4) | C15—C16—C17—N6 | −177.4 (4) |
C2i—C3—C4—C5i | −39.5 (4) | O1—C12—C17—C16 | −178.8 (4) |
C2—C3—C4—C5i | 140.5 (4) | O1—C12—C17—N6 | −1.7 (5) |
C5i—C4—C5—C6 | 0.5 (4) | C13—C12—C17—N6 | 177.1 (5) |
C3—C4—C5—C6 | −179.5 (4) | O7—N6—C17—C16 | −172.6 (7) |
C6i—N2—C6—C5 | 0.6 (4) | O6—N6—C17—C16 | 9.7 (8) |
Zn1iv—N2—C6—C5 | −179.4 (4) | O7—N6—C17—C12 | 10 (1) |
C4—C5—C6—N2 | −1.2 (8) | O6—N6—C17—C12 | −167.6 (6) |
Symmetry codes: (i) −x+1, y, −z+1/2; (ii) x, y−1, z; (iii) −x+1, −y+1, −z+1; (iv) x, y+1, z. |
D—H···A | D—H | H···A | D···A | D—H···A |
O1w—H1w1···O2w | 0.85 (1) | 1.89 (1) | 2.731 (5) | 169 (5) |
O1w—H1w2···O1 | 0.85 (1) | 1.86 (2) | 2.695 (5) | 168 (6) |
O2w—H2w1···O3v | 0.85 (1) | 2.27 (3) | 3.064 (7) | 155 (5) |
O2w—H2w2···O7vi | 0.85 (1) | 2.34 (4) | 2.949 (8) | 128 (4) |
Symmetry codes: (v) −x+1/2, y−1/2, −z+1/2; (vi) −x+1/2, y+1/2, −z+1/2. |
Experimental details
Crystal data | |
Chemical formula | [Zn(C10H8N2)2(H2O)2](C6H2N3O7)2·2H2O |
Mr | 906.01 |
Crystal system, space group | Monoclinic, C2/c |
Temperature (K) | 298 |
a, b, c (Å) | 14.391 (2), 11.418 (1), 22.908 (3) |
β (°) | 95.08 (1) |
V (Å3) | 3749.4 (8) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 0.75 |
Crystal size (mm) | 0.18 × 0.15 × 0.12 |
Data collection | |
Diffractometer | Enraf-Nonius CAD-4 diffractometer |
Absorption correction | Empirical VIA ψ scan (North et al., 1968) |
Tmin, Tmax | 0.874, 0.914 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 3829, 3679, 2020 |
Rint | 0.021 |
(sin θ/λ)max (Å−1) | 0.617 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.057, 0.152, 1.01 |
No. of reflections | 3679 |
No. of parameters | 278 |
No. of restraints | 24 |
H-atom treatment | H atoms treated by a mixture of independent and constrained refinement |
Δρmax, Δρmin (e Å−3) | 0.61, −0.60 |
Computer programs: CAD-4 Software (Enraf-Nonius, 1988), CAD-4 Software, XCAD4 (Harms, 1997), SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), ORTEPII (Johnson, 1976), SHELXL97.
The reaction of zinc dipicrate octahydrate with 4,4'-bipyridine gives bis(4,4'-bipyridine)diaquazinc dipicrate (Liang et al., 2000) as a dihydrate (Liang et al., 2001b), (I), as well as a monohydrated co-crystal with 4,4'-bipyridine (Liang et al., 2001a). The crystal structures of both were refined in the Cc space group; that of the dihydrate was refined to 0.087 for 2584 I > σ(I) reflections. However, the published packing diagram shows a centric arrangement of the contents. In the revised C2/c setting, the structure refined to 0.057, but some retraints had to be imposed to the model (Fig. 1). In the revised description, the Zn atom lies on a twofold axis as does one of the two 4,4-bipyridine units. This axis passes through the two N atoms. The other spacer unit lies on an inversion center that is mid-way between the 4- and 4'-carbon atoms. Arising from the revision, the 4,4'-bipyridine–zinc layer motif is better regarded as an almost perfect square. One side is the b-axial distance whereas the other is half the c axis, as seen from the axial ratio (11.418 Å/22.908 Å) that is nearly 1/2.