Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807032692/wn2163sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536807032692/wn2163Isup2.hkl |
CCDC reference: 657553
Key indicators
- Single-crystal X-ray study
- T = 273 K
- Mean (C-C) = 0.004 Å
- R factor = 0.025
- wR factor = 0.054
- Data-to-parameter ratio = 11.4
checkCIF/PLATON results
No syntax errors found
Alert level C PLAT062_ALERT_4_C Rescale T(min) & T(max) by ..................... 0.97 PLAT143_ALERT_4_C su on c - Axis Small or Missing (x 100000) ..... 10 Ang. PLAT180_ALERT_3_C Check Cell Rounding: # of Values Ending with 0 = 3 PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Zn1 - O2 .. 6.33 su PLAT764_ALERT_4_C Overcomplete CIF Bond List Detected (Rep/Expd) . 1.12 Ratio
Alert level G PLAT794_ALERT_5_G Check Predicted Bond Valency for Zn1 (2) 2.20
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 5 ALERT level C = Check and explain 1 ALERT level G = General alerts; check 0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 1 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 3 ALERT type 4 Improvement, methodology, query or suggestion 1 ALERT type 5 Informative message, check
A mixture of ZnSO3 (0.145 g, 1 mmol), 2,2'-bipyridine (0.168 g, 1 mmol) and H2O (18 ml) was sealed in a 25 ml Teflon-lined stainless steel reactor and was heated at 373 K for 3 d. On completion of the reaction, the reactor was cooled slowly to room temperature and the mixture was filtered, giving colorless single crystals suitable for X-ray analysis.
All H atoms were placed at calculated positions, and refined using a riding model [C—H = 0.93Å and Uiso(H) = 1.2Ueq(C)].
Metal organic frameworks based on the SO32- unit are of current interest (Nguyen et al., 2006). We report here a new zinc sulfite structure, Zn2(SO3)2(2,2'-bipyridine)2.
In the title compound, Zn2+ and SO32- form an dinuclear unit, with an inversion center at the mid-point of the Zn···Zn vector (Fig.1). Each Zn atom has distorted octahedral geometry and is coordinated by four O atoms from two different SO32- anions and two N atoms from the 2,2'-bipyridine ligand. It is worth noting that Zn1 and Zn1a share two common oxygen sites from two SO32- anions. In the SO32- group, one oxygen site is linked to two Zn2+ and one S4+ sites; the other two oxygen sites are each linked to one Zn2+ and one S4+ sites. The 2,2'-bipyridine ligands chelate the Zn sites.
For related literature, see: Nguyen et al. (2006).
Data collection: SMART (Siemens, 1996); cell refinement: SAINT (Siemens, 1996); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Siemens, 1996); software used to prepare material for publication: SHELXTL.
Fig. 1. The molecular structure of the title compound, showing 50% probability displacement ellipsoids [symmetry code: (a) -x,-y,-z]. |
[Zn2(SO3)2(C10H8N2)2] | Z = 2 |
Mr = 603.23 | F(000) = 608 |
Monoclinic, P21/n | Dx = 1.923 Mg m−3 |
Hall symbol: -P2yn | Mo Kα radiation, λ = 0.71073 Å |
a = 8.1444 (1) Å | θ = 2.6–25.0° |
b = 13.2118 (2) Å | µ = 2.55 mm−1 |
c = 10.3020 (1) Å | T = 273 K |
β = 109.970 (1)° | Prism, colorless |
V = 1041.86 (2) Å3 | 0.21 × 0.13 × 0.10 mm |
Siemens SMART 1K CCD area-detector diffractometer | 1756 independent reflections |
Radiation source: fine-focus sealed tube | 1413 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.055 |
φ and ω scans | θmax = 25.0°, θmin = 2.6° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −9→9 |
Tmin = 0.700, Tmax = 0.800 | k = −15→15 |
8021 measured reflections | l = −12→12 |
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) = 0.054 | H-atom parameters constrained |
S = 0.94 | w = 1/[σ2(Fo2) + (0.0226P)2] where P = (Fo2 + 2Fc2)/3 |
1756 reflections | (Δ/σ)max < 0.001 |
154 parameters | Δρmax = 0.34 e Å−3 |
0 restraints | Δρmin = −0.46 e Å−3 |
[Zn2(SO3)2(C10H8N2)2] | V = 1041.86 (2) Å3 |
Mr = 603.23 | Z = 2 |
Monoclinic, P21/n | Mo Kα radiation |
a = 8.1444 (1) Å | µ = 2.55 mm−1 |
b = 13.2118 (2) Å | T = 273 K |
c = 10.3020 (1) Å | 0.21 × 0.13 × 0.10 mm |
β = 109.970 (1)° |
Siemens SMART 1K CCD area-detector diffractometer | 1756 independent reflections |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | 1413 reflections with I > 2σ(I) |
Tmin = 0.700, Tmax = 0.800 | Rint = 0.055 |
8021 measured reflections |
R[F2 > 2σ(F2)] = 0.025 | 0 restraints |
wR(F2) = 0.054 | H-atom parameters constrained |
S = 0.94 | Δρmax = 0.34 e Å−3 |
1756 reflections | Δρmin = −0.46 e Å−3 |
154 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 | ||
Zn1 | 0.07078 (4) | 0.00807 (2) | 0.16944 (3) | 0.01426 (11) | |
S1 | 0.27778 (9) | −0.00925 (5) | 0.00581 (7) | 0.01588 (17) | |
O2 | 0.1343 (2) | −0.08446 (12) | 0.01526 (18) | 0.0166 (4) | |
N2 | 0.0632 (3) | 0.11128 (15) | 0.3230 (2) | 0.0141 (5) | |
N1 | 0.2190 (3) | −0.06780 (14) | 0.3510 (2) | 0.0135 (5) | |
O1 | 0.2832 (2) | 0.06485 (13) | 0.12097 (18) | 0.0188 (4) | |
C6 | 0.1471 (3) | 0.08117 (18) | 0.4537 (3) | 0.0127 (6) | |
C5 | 0.3016 (4) | −0.15614 (19) | 0.3572 (3) | 0.0177 (6) | |
H5A | 0.2819 | −0.1922 | 0.2758 | 0.021* | |
C4 | 0.1365 (4) | 0.13747 (19) | 0.5649 (3) | 0.0179 (6) | |
H4A | 0.1936 | 0.1159 | 0.6550 | 0.021* | |
C3 | −0.0344 (4) | 0.19588 (18) | 0.3002 (3) | 0.0172 (6) | |
H3A | −0.0953 | 0.2149 | 0.2096 | 0.021* | |
C2 | 0.4143 (4) | −0.1964 (2) | 0.4782 (3) | 0.0202 (7) | |
H2A | 0.4680 | −0.2587 | 0.4793 | 0.024* | |
C1 | 0.2462 (3) | −0.01508 (18) | 0.4696 (3) | 0.0131 (6) | |
O3 | 0.1804 (3) | 0.04415 (13) | −0.13110 (18) | 0.0186 (4) | |
C10 | 0.4447 (4) | −0.14091 (19) | 0.5983 (3) | 0.0201 (7) | |
H10A | 0.5227 | −0.1647 | 0.6815 | 0.024* | |
C9 | −0.0478 (4) | 0.25539 (19) | 0.4057 (3) | 0.0199 (7) | |
H9A | −0.1145 | 0.3142 | 0.3870 | 0.024* | |
C8 | 0.0400 (4) | 0.22563 (19) | 0.5396 (3) | 0.0203 (7) | |
H8A | 0.0343 | 0.2649 | 0.6128 | 0.024* | |
C7 | 0.3591 (4) | −0.05038 (19) | 0.5940 (3) | 0.0177 (6) | |
H7A | 0.3772 | −0.0133 | 0.6744 | 0.021* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Zn1 | 0.01481 (19) | 0.01848 (17) | 0.00850 (19) | −0.00008 (14) | 0.00271 (16) | −0.00131 (13) |
S1 | 0.0132 (4) | 0.0205 (3) | 0.0136 (4) | −0.0016 (3) | 0.0043 (3) | 0.0005 (3) |
O2 | 0.0164 (11) | 0.0184 (9) | 0.0146 (11) | −0.0031 (8) | 0.0046 (10) | 0.0002 (8) |
N2 | 0.0130 (14) | 0.0178 (11) | 0.0102 (13) | −0.0021 (9) | 0.0024 (12) | −0.0007 (9) |
N1 | 0.0133 (13) | 0.0173 (11) | 0.0102 (13) | −0.0029 (9) | 0.0044 (11) | −0.0037 (9) |
O1 | 0.0209 (12) | 0.0238 (10) | 0.0104 (11) | −0.0070 (8) | 0.0036 (10) | −0.0026 (8) |
C6 | 0.0116 (15) | 0.0152 (13) | 0.0112 (16) | −0.0032 (11) | 0.0039 (14) | −0.0008 (10) |
C5 | 0.0193 (17) | 0.0200 (14) | 0.0144 (17) | 0.0009 (12) | 0.0067 (15) | −0.0026 (11) |
C4 | 0.0215 (17) | 0.0213 (14) | 0.0107 (16) | −0.0026 (12) | 0.0054 (15) | −0.0022 (11) |
C3 | 0.0165 (17) | 0.0182 (13) | 0.0156 (17) | 0.0027 (11) | 0.0038 (15) | 0.0038 (11) |
C2 | 0.0211 (18) | 0.0197 (14) | 0.0212 (18) | 0.0046 (12) | 0.0091 (16) | 0.0031 (12) |
C1 | 0.0117 (15) | 0.0175 (13) | 0.0108 (15) | −0.0040 (11) | 0.0047 (14) | 0.0007 (11) |
O3 | 0.0195 (12) | 0.0257 (10) | 0.0094 (11) | −0.0042 (8) | 0.0034 (10) | 0.0020 (8) |
C10 | 0.0175 (18) | 0.0249 (15) | 0.0146 (17) | −0.0003 (12) | 0.0013 (15) | 0.0069 (12) |
C9 | 0.0212 (18) | 0.0154 (13) | 0.0254 (18) | 0.0011 (12) | 0.0108 (16) | −0.0019 (12) |
C8 | 0.0231 (19) | 0.0210 (14) | 0.0192 (18) | −0.0045 (12) | 0.0101 (16) | −0.0083 (12) |
C7 | 0.0200 (18) | 0.0226 (14) | 0.0096 (16) | −0.0034 (12) | 0.0040 (15) | −0.0007 (11) |
Zn1—O3i | 2.0651 (19) | C6—C1 | 1.485 (3) |
Zn1—O1 | 2.0963 (17) | C5—C2 | 1.378 (4) |
Zn1—N1 | 2.102 (2) | C5—H5A | 0.9300 |
Zn1—N2 | 2.105 (2) | C4—C8 | 1.379 (4) |
Zn1—O2 | 2.2016 (16) | C4—H4A | 0.9300 |
Zn1—O2i | 2.2932 (19) | C3—C9 | 1.375 (3) |
Zn1—S1 | 2.7708 (6) | C3—H3A | 0.9300 |
Zn1—S1i | 2.7961 (8) | C2—C10 | 1.386 (4) |
S1—O1 | 1.5271 (17) | C2—H2A | 0.9300 |
S1—O3 | 1.5337 (19) | C1—C7 | 1.378 (4) |
S1—O2 | 1.5618 (18) | O3—Zn1i | 2.0651 (19) |
S1—Zn1i | 2.7961 (8) | C10—C7 | 1.378 (4) |
O2—Zn1i | 2.2932 (19) | C10—H10A | 0.9300 |
N2—C6 | 1.345 (3) | C9—C8 | 1.377 (4) |
N2—C3 | 1.345 (3) | C9—H9A | 0.9300 |
N1—C5 | 1.337 (3) | C8—H8A | 0.9300 |
N1—C1 | 1.357 (3) | C7—H7A | 0.9300 |
C6—C4 | 1.393 (3) | ||
O3i—Zn1—O1 | 156.65 (7) | Zn1—O2—Zn1i | 94.02 (7) |
O3i—Zn1—N1 | 103.97 (7) | C6—N2—C3 | 119.2 (2) |
O1—Zn1—N1 | 96.46 (7) | C6—N2—Zn1 | 115.17 (16) |
O3i—Zn1—N2 | 94.52 (8) | C3—N2—Zn1 | 125.06 (19) |
O1—Zn1—N2 | 100.69 (7) | C5—N1—C1 | 118.7 (2) |
N1—Zn1—N2 | 78.21 (8) | C5—N1—Zn1 | 125.85 (18) |
O3i—Zn1—O2 | 97.94 (7) | C1—N1—Zn1 | 115.07 (16) |
O1—Zn1—O2 | 67.07 (6) | S1—O1—Zn1 | 98.54 (9) |
N1—Zn1—O2 | 99.90 (7) | N2—C6—C4 | 120.8 (2) |
N2—Zn1—O2 | 167.47 (8) | N2—C6—C1 | 115.8 (2) |
O3i—Zn1—O2i | 66.11 (6) | C4—C6—C1 | 123.4 (2) |
O1—Zn1—O2i | 94.10 (7) | N1—C5—C2 | 123.3 (2) |
N1—Zn1—O2i | 169.26 (7) | N1—C5—H5A | 118.3 |
N2—Zn1—O2i | 97.96 (7) | C2—C5—H5A | 118.3 |
O2—Zn1—O2i | 85.98 (7) | C8—C4—C6 | 119.1 (3) |
O3i—Zn1—S1 | 128.67 (5) | C8—C4—H4A | 120.4 |
O1—Zn1—S1 | 33.03 (5) | C6—C4—H4A | 120.4 |
N1—Zn1—S1 | 102.59 (6) | N2—C3—C9 | 122.6 (3) |
N2—Zn1—S1 | 133.68 (6) | N2—C3—H3A | 118.7 |
O2—Zn1—S1 | 34.25 (5) | C9—C3—H3A | 118.7 |
O2i—Zn1—S1 | 87.35 (4) | C5—C2—C10 | 117.7 (2) |
O3i—Zn1—S1i | 32.58 (5) | C5—C2—H2A | 121.2 |
O1—Zn1—S1i | 125.64 (5) | C10—C2—H2A | 121.2 |
N1—Zn1—S1i | 136.49 (6) | N1—C1—C7 | 121.0 (2) |
N2—Zn1—S1i | 101.41 (6) | N1—C1—C6 | 115.1 (2) |
O2—Zn1—S1i | 88.53 (5) | C7—C1—C6 | 123.8 (2) |
O2i—Zn1—S1i | 33.95 (4) | S1—O3—Zn1i | 100.93 (8) |
S1—Zn1—S1i | 107.589 (18) | C7—C10—C2 | 119.7 (3) |
O1—S1—O3 | 106.75 (10) | C7—C10—H10A | 120.1 |
O1—S1—O2 | 100.56 (9) | C2—C10—H10A | 120.1 |
O3—S1—O2 | 100.78 (10) | C3—C9—C8 | 118.3 (2) |
O1—S1—Zn1 | 48.44 (7) | C3—C9—H9A | 120.9 |
O3—S1—Zn1 | 106.88 (7) | C8—C9—H9A | 120.9 |
O2—S1—Zn1 | 52.49 (6) | C9—C8—C4 | 119.9 (2) |
O1—S1—Zn1i | 104.57 (8) | C9—C8—H8A | 120.1 |
O3—S1—Zn1i | 46.48 (7) | C4—C8—H8A | 120.1 |
O2—S1—Zn1i | 55.09 (7) | C10—C7—C1 | 119.6 (2) |
Zn1—S1—Zn1i | 72.411 (18) | C10—C7—H7A | 120.2 |
S1—O2—Zn1 | 93.26 (8) | C1—C7—H7A | 120.2 |
S1—O2—Zn1i | 90.96 (8) |
Symmetry code: (i) −x, −y, −z. |
Experimental details
Crystal data | |
Chemical formula | [Zn2(SO3)2(C10H8N2)2] |
Mr | 603.23 |
Crystal system, space group | Monoclinic, P21/n |
Temperature (K) | 273 |
a, b, c (Å) | 8.1444 (1), 13.2118 (2), 10.3020 (1) |
β (°) | 109.970 (1) |
V (Å3) | 1041.86 (2) |
Z | 2 |
Radiation type | Mo Kα |
µ (mm−1) | 2.55 |
Crystal size (mm) | 0.21 × 0.13 × 0.10 |
Data collection | |
Diffractometer | Siemens SMART 1K CCD area-detector |
Absorption correction | Multi-scan (SADABS; Sheldrick, 1996) |
Tmin, Tmax | 0.700, 0.800 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 8021, 1756, 1413 |
Rint | 0.055 |
(sin θ/λ)max (Å−1) | 0.596 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.025, 0.054, 0.94 |
No. of reflections | 1756 |
No. of parameters | 154 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 0.34, −0.46 |
Computer programs: SMART (Siemens, 1996), SAINT (Siemens, 1996), SAINT, SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), SHELXTL (Siemens, 1996), SHELXTL.
Zn1—O3i | 2.0651 (19) | Zn1—N2 | 2.105 (2) |
Zn1—O1 | 2.0963 (17) | Zn1—O2 | 2.2016 (16) |
Zn1—N1 | 2.102 (2) | Zn1—O2i | 2.2932 (19) |
O3i—Zn1—O1 | 156.65 (7) | N1—Zn1—O2 | 99.90 (7) |
O3i—Zn1—N1 | 103.97 (7) | N2—Zn1—O2 | 167.47 (8) |
O1—Zn1—N1 | 96.46 (7) | O3i—Zn1—O2i | 66.11 (6) |
O3i—Zn1—N2 | 94.52 (8) | O1—Zn1—O2i | 94.10 (7) |
O1—Zn1—N2 | 100.69 (7) | N1—Zn1—O2i | 169.26 (7) |
N1—Zn1—N2 | 78.21 (8) | N2—Zn1—O2i | 97.96 (7) |
O3i—Zn1—O2 | 97.94 (7) | O2—Zn1—O2i | 85.98 (7) |
O1—Zn1—O2 | 67.07 (6) |
Symmetry code: (i) −x, −y, −z. |
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Metal organic frameworks based on the SO32- unit are of current interest (Nguyen et al., 2006). We report here a new zinc sulfite structure, Zn2(SO3)2(2,2'-bipyridine)2.
In the title compound, Zn2+ and SO32- form an dinuclear unit, with an inversion center at the mid-point of the Zn···Zn vector (Fig.1). Each Zn atom has distorted octahedral geometry and is coordinated by four O atoms from two different SO32- anions and two N atoms from the 2,2'-bipyridine ligand. It is worth noting that Zn1 and Zn1a share two common oxygen sites from two SO32- anions. In the SO32- group, one oxygen site is linked to two Zn2+ and one S4+ sites; the other two oxygen sites are each linked to one Zn2+ and one S4+ sites. The 2,2'-bipyridine ligands chelate the Zn sites.