Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807058539/at2479sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536807058539/at2479Isup2.hkl |
CCDC reference: 672780
Key indicators
- Single-crystal X-ray study
- T = 296 K
- Mean (Wav) = 0.000 Å
- R factor = 0.016
- wR factor = 0.042
- Data-to-parameter ratio = 14.7
checkCIF/PLATON results
No syntax errors found
Alert level G 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 0.914 Tmax scaled 0.743 Tmin scaled 0.574
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 0 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 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 0 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check
For related literature, see: Chen et al. (1998); He & Feng (2007); Shuai et al. (2007); Zhang et al. (2006).
A solution of BaCl2 (0.2497 g, 1 mmol) and H2CCOP (0.2025 g, 1 mmol) was mixed and stirred at room temperature. Then the mixture was stood at ambient temperature. By slow evaporation of the solvent, well formed colourless crystals, suitable for X-ray analysis were obtained after two days.
The H atoms bonded to C atoms were positioned geometrically and allowed to ride on their parent atoms, with C—H = 0.93 and 0.97 Å, and Uiso=1.2Ueq (C). The H atoms bonded to O atoms were located in a difference Fourier maps and refined freely.
Data collection: APEX2 (Bruker, 2004); cell refinement: SAINT (Bruker, 2004); data reduction: SAINT (Bruker, 2004); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Bruker, 2002); software used to prepare material for publication: SHELXL97 (Sheldrick, 1997).
[Ba(C8H5NO5)(H2O)5] | Z = 2 |
Mr = 422.55 | F(000) = 412 |
Triclinic, P1 | Dx = 2.061 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71073 Å |
a = 7.0051 (14) Å | Cell parameters from 11388 reflections |
b = 9.7371 (19) Å | θ = 2.0–27.5° |
c = 11.201 (2) Å | µ = 2.97 mm−1 |
α = 112.88 (3)° | T = 296 K |
β = 95.63 (3)° | Block, colourless |
γ = 100.18 (3)° | 0.16 × 0.14 × 0.10 mm |
V = 681.0 (2) Å3 |
Bruker APEXII area-detector diffractometer | 3104 independent reflections |
Radiation source: fine-focus sealed tube | 2971 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.023 |
ω scans | θmax = 27.5°, θmin = 2.0° |
Absorption correction: empirical (using intensity measurements) (SADABS; Sheldrick, 1996) | h = −9→9 |
Tmin = 0.628, Tmax = 0.813 | k = −12→12 |
11353 measured reflections | l = −14→14 |
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)] = 0.016 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.042 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.01 | w = 1/[σ2(Fo2) + (0.0265P)2 + 0.162P] where P = (Fo2 + 2Fc2)/3 |
3104 reflections | (Δ/σ)max = 0.003 |
211 parameters | Δρmax = 0.58 e Å−3 |
15 restraints | Δρmin = −0.45 e Å−3 |
[Ba(C8H5NO5)(H2O)5] | γ = 100.18 (3)° |
Mr = 422.55 | V = 681.0 (2) Å3 |
Triclinic, P1 | Z = 2 |
a = 7.0051 (14) Å | Mo Kα radiation |
b = 9.7371 (19) Å | µ = 2.97 mm−1 |
c = 11.201 (2) Å | T = 296 K |
α = 112.88 (3)° | 0.16 × 0.14 × 0.10 mm |
β = 95.63 (3)° |
Bruker APEXII area-detector diffractometer | 3104 independent reflections |
Absorption correction: empirical (using intensity measurements) (SADABS; Sheldrick, 1996) | 2971 reflections with I > 2σ(I) |
Tmin = 0.628, Tmax = 0.813 | Rint = 0.023 |
11353 measured reflections |
R[F2 > 2σ(F2)] = 0.016 | 15 restraints |
wR(F2) = 0.042 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.01 | Δρmax = 0.58 e Å−3 |
3104 reflections | Δρmin = −0.45 e Å−3 |
211 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 | ||
Ba | 0.600166 (14) | 0.757213 (11) | 0.602839 (10) | 0.02020 (5) | |
O1 | 0.4232 (3) | 0.72415 (16) | 0.35817 (16) | 0.0381 (4) | |
O1W | 0.1915 (2) | 0.69116 (18) | 0.61729 (16) | 0.0341 (3) | |
H1WA | 0.134 (4) | 0.748 (3) | 0.6738 (19) | 0.041* | |
H1WB | 0.109 (3) | 0.672 (3) | 0.5494 (17) | 0.041* | |
O2 | 0.3509 (2) | 0.49709 (16) | 0.36455 (14) | 0.0304 (3) | |
O2W | 0.8518 (2) | 0.62065 (18) | 0.43111 (15) | 0.0339 (3) | |
H2WA | 0.867 (4) | 0.645 (3) | 0.371 (2) | 0.041* | |
H2WB | 0.825 (4) | 0.5260 (19) | 0.401 (2) | 0.041* | |
O3 | 0.0848 (3) | 0.28461 (19) | −0.23870 (15) | 0.0426 (4) | |
O3W | 0.4998 (3) | 0.8244 (2) | 0.85769 (16) | 0.0448 (4) | |
H3WA | 0.572 (4) | 0.856 (3) | 0.929 (2) | 0.054* | |
H3WB | 0.415 (3) | 0.879 (3) | 0.871 (3) | 0.054* | |
O4 | 0.2545 (2) | 0.04168 (17) | −0.10934 (15) | 0.0330 (3) | |
O4W | 0.8181 (3) | 0.9993 (2) | 0.5519 (2) | 0.0471 (4) | |
H4WA | 0.929 (3) | 1.000 (3) | 0.545 (3) | 0.057* | |
H4WB | 0.805 (4) | 1.083 (2) | 0.592 (3) | 0.057* | |
O5 | −0.0335 (2) | −0.11523 (16) | −0.22398 (15) | 0.0321 (3) | |
O5W | 0.4634 (4) | 1.0222 (2) | 0.6837 (2) | 0.0610 (6) | |
H5WA | 0.494 (5) | 1.105 (3) | 0.677 (3) | 0.073* | |
H5WB | 0.404 (5) | 1.038 (4) | 0.745 (3) | 0.073* | |
N1 | 0.0942 (2) | 0.29402 (17) | −0.03292 (15) | 0.0224 (3) | |
C6 | 0.3557 (3) | 0.5812 (2) | 0.30310 (19) | 0.0243 (4) | |
C1 | 0.1429 (3) | 0.3611 (2) | −0.11786 (19) | 0.0265 (4) | |
C7 | −0.0354 (3) | 0.1403 (2) | −0.0908 (2) | 0.0249 (4) | |
H7A | −0.1350 | 0.1337 | −0.1606 | 0.030* | |
H7B | −0.1026 | 0.1245 | −0.0239 | 0.030* | |
C4 | 0.2792 (3) | 0.5095 (2) | 0.15796 (19) | 0.0232 (4) | |
C2 | 0.2571 (3) | 0.5157 (2) | −0.0563 (2) | 0.0276 (4) | |
H2 | 0.2876 | 0.5688 | −0.1079 | 0.033* | |
C3 | 0.3217 (3) | 0.5864 (2) | 0.0757 (2) | 0.0265 (4) | |
H3 | 0.3953 | 0.6873 | 0.1131 | 0.032* | |
C8 | 0.0716 (3) | 0.0126 (2) | −0.14697 (18) | 0.0227 (4) | |
C5 | 0.1647 (3) | 0.3642 (2) | 0.09955 (18) | 0.0227 (4) | |
H5 | 0.1336 | 0.3113 | 0.1513 | 0.027* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Ba | 0.02295 (7) | 0.01711 (6) | 0.01811 (7) | 0.00351 (4) | 0.00071 (4) | 0.00599 (5) |
O1 | 0.0590 (10) | 0.0203 (7) | 0.0255 (7) | −0.0028 (7) | −0.0107 (7) | 0.0091 (6) |
O1W | 0.0306 (8) | 0.0331 (8) | 0.0303 (8) | 0.0070 (6) | 0.0020 (6) | 0.0055 (7) |
O2 | 0.0442 (8) | 0.0217 (7) | 0.0233 (7) | 0.0038 (6) | −0.0015 (6) | 0.0107 (6) |
O2W | 0.0442 (9) | 0.0325 (8) | 0.0268 (8) | 0.0097 (7) | 0.0085 (7) | 0.0134 (7) |
O3 | 0.0636 (11) | 0.0370 (9) | 0.0190 (8) | 0.0019 (8) | 0.0028 (7) | 0.0084 (7) |
O3W | 0.0505 (10) | 0.0552 (11) | 0.0252 (8) | 0.0262 (9) | 0.0016 (7) | 0.0084 (8) |
O4 | 0.0271 (7) | 0.0337 (8) | 0.0299 (8) | 0.0104 (6) | −0.0023 (6) | 0.0050 (6) |
O4W | 0.0495 (10) | 0.0400 (9) | 0.0489 (11) | 0.0050 (8) | 0.0125 (9) | 0.0169 (9) |
O5 | 0.0356 (8) | 0.0198 (7) | 0.0314 (8) | 0.0032 (6) | −0.0006 (6) | 0.0037 (6) |
O5W | 0.0873 (15) | 0.0316 (9) | 0.0900 (17) | 0.0288 (10) | 0.0619 (13) | 0.0353 (10) |
N1 | 0.0264 (8) | 0.0189 (7) | 0.0201 (8) | 0.0063 (6) | 0.0021 (6) | 0.0061 (6) |
C6 | 0.0275 (9) | 0.0221 (9) | 0.0210 (9) | 0.0048 (7) | −0.0005 (7) | 0.0082 (7) |
C1 | 0.0333 (10) | 0.0279 (10) | 0.0184 (9) | 0.0105 (8) | 0.0036 (8) | 0.0086 (8) |
C7 | 0.0244 (9) | 0.0206 (9) | 0.0237 (10) | 0.0029 (7) | 0.0002 (7) | 0.0048 (7) |
C4 | 0.0256 (9) | 0.0213 (9) | 0.0214 (9) | 0.0067 (7) | 0.0019 (7) | 0.0077 (7) |
C2 | 0.0339 (10) | 0.0281 (10) | 0.0254 (10) | 0.0083 (8) | 0.0065 (8) | 0.0152 (8) |
C3 | 0.0271 (10) | 0.0222 (9) | 0.0299 (11) | 0.0052 (7) | 0.0025 (8) | 0.0113 (8) |
C8 | 0.0280 (9) | 0.0236 (9) | 0.0163 (9) | 0.0066 (7) | 0.0019 (7) | 0.0084 (7) |
C5 | 0.0275 (9) | 0.0221 (9) | 0.0198 (9) | 0.0083 (7) | 0.0034 (7) | 0.0091 (7) |
Ba—O2i | 2.7132 (15) | O4—C8 | 1.254 (2) |
Ba—O5W | 2.7609 (19) | O4W—H4WA | 0.787 (16) |
Ba—O1 | 2.7673 (17) | O4W—H4WB | 0.793 (16) |
Ba—O5ii | 2.8129 (19) | O5—C8 | 1.246 (2) |
Ba—O2W | 2.8424 (18) | O5—Baiii | 2.8129 (19) |
Ba—O1W | 2.8560 (17) | O5W—H5WA | 0.831 (17) |
Ba—O4W | 2.856 (2) | O5W—H5WB | 0.812 (17) |
Ba—O3W | 2.8593 (19) | N1—C5 | 1.364 (2) |
Ba—O2 | 2.976 (2) | N1—C1 | 1.384 (3) |
Ba—C6 | 3.241 (2) | N1—C7 | 1.461 (2) |
Ba—Bai | 4.5027 (17) | C6—C4 | 1.494 (3) |
O1—C6 | 1.259 (2) | C1—C2 | 1.429 (3) |
O1W—H1WA | 0.855 (16) | C7—C8 | 1.522 (3) |
O1W—H1WB | 0.844 (16) | C7—H7A | 0.9700 |
O2—C6 | 1.256 (2) | C7—H7B | 0.9700 |
O2—Bai | 2.7132 (15) | C4—C5 | 1.359 (3) |
O2W—H2WA | 0.804 (16) | C4—C3 | 1.418 (3) |
O2W—H2WB | 0.826 (16) | C2—C3 | 1.354 (3) |
O3—C1 | 1.246 (2) | C2—H2 | 0.9300 |
O3W—H3WA | 0.818 (17) | C3—H3 | 0.9300 |
O3W—H3WB | 0.852 (17) | C5—H5 | 0.9300 |
O2i—Ba—O5W | 149.47 (5) | C6—Ba—Bai | 57.41 (5) |
O2i—Ba—O1 | 118.73 (5) | C6—O1—Ba | 100.42 (12) |
O5W—Ba—O1 | 81.72 (7) | Ba—O1W—H1WA | 126.3 (17) |
O2i—Ba—O5ii | 81.75 (5) | Ba—O1W—H1WB | 117.4 (17) |
O5W—Ba—O5ii | 96.55 (7) | H1WA—O1W—H1WB | 97.3 (19) |
O1—Ba—O5ii | 140.28 (5) | C6—O2—Bai | 153.83 (13) |
O2i—Ba—O2W | 71.99 (5) | C6—O2—Ba | 90.53 (11) |
O5W—Ba—O2W | 137.98 (5) | Bai—O2—Ba | 104.56 (5) |
O1—Ba—O2W | 75.98 (6) | Ba—O2W—H2WA | 118.5 (19) |
O5ii—Ba—O2W | 79.65 (5) | Ba—O2W—H2WB | 114.0 (19) |
O2i—Ba—O1W | 91.48 (5) | H2WA—O2W—H2WB | 107 (2) |
O5W—Ba—O1W | 69.51 (6) | Ba—O3W—H3WA | 129 (2) |
O1—Ba—O1W | 78.36 (6) | Ba—O3W—H3WB | 111 (2) |
O5ii—Ba—O1W | 138.31 (5) | H3WA—O3W—H3WB | 104 (2) |
O2W—Ba—O1W | 137.03 (5) | Ba—O4W—H4WA | 118 (2) |
O2i—Ba—O4W | 139.77 (5) | Ba—O4W—H4WB | 118 (2) |
O5W—Ba—O4W | 64.80 (6) | H4WA—O4W—H4WB | 111 (2) |
O1—Ba—O4W | 73.10 (6) | C8—O5—Baiii | 139.64 (13) |
O5ii—Ba—O4W | 70.48 (6) | Ba—O5W—H5WA | 135 (2) |
O2W—Ba—O4W | 74.76 (6) | Ba—O5W—H5WB | 116 (2) |
O1W—Ba—O4W | 128.59 (6) | H5WA—O5W—H5WB | 106 (2) |
O2i—Ba—O3W | 79.46 (6) | C5—N1—C1 | 122.79 (16) |
O5W—Ba—O3W | 70.65 (6) | C5—N1—C7 | 119.92 (16) |
O1—Ba—O3W | 137.63 (6) | C1—N1—C7 | 117.28 (16) |
O5ii—Ba—O3W | 76.00 (6) | O2—C6—O1 | 122.98 (18) |
O2W—Ba—O3W | 144.67 (5) | O2—C6—C4 | 119.01 (17) |
O1W—Ba—O3W | 62.34 (6) | O1—C6—C4 | 118.01 (17) |
O4W—Ba—O3W | 119.19 (6) | O2—C6—Ba | 66.66 (10) |
O2i—Ba—O2 | 75.44 (5) | O1—C6—Ba | 57.12 (11) |
O5W—Ba—O2 | 114.74 (7) | C4—C6—Ba | 169.13 (13) |
O1—Ba—O2 | 45.08 (4) | O3—C1—N1 | 118.76 (18) |
O5ii—Ba—O2 | 147.62 (5) | O3—C1—C2 | 125.75 (19) |
O2W—Ba—O2 | 71.66 (5) | N1—C1—C2 | 115.48 (17) |
O1W—Ba—O2 | 65.78 (5) | N1—C7—C8 | 113.86 (16) |
O4W—Ba—O2 | 114.43 (5) | N1—C7—H7A | 108.8 |
O3W—Ba—O2 | 120.87 (6) | C8—C7—H7A | 108.8 |
O2i—Ba—C6 | 96.73 (5) | N1—C7—H7B | 108.8 |
O5W—Ba—C6 | 99.81 (7) | C8—C7—H7B | 108.8 |
O1—Ba—C6 | 22.46 (4) | H7A—C7—H7B | 107.7 |
O5ii—Ba—C6 | 148.80 (5) | C5—C4—C3 | 117.30 (18) |
O2W—Ba—C6 | 70.40 (5) | C5—C4—C6 | 119.97 (18) |
O1W—Ba—C6 | 72.70 (6) | C3—C4—C6 | 122.73 (17) |
O4W—Ba—C6 | 92.84 (6) | C3—C2—C1 | 121.25 (18) |
O3W—Ba—C6 | 134.65 (6) | C3—C2—H2 | 119.4 |
O2—Ba—C6 | 22.81 (4) | C1—C2—H2 | 119.4 |
O2i—Ba—Bai | 39.76 (3) | C2—C3—C4 | 121.21 (18) |
O5W—Ba—Bai | 142.72 (5) | C2—C3—H3 | 119.4 |
O1—Ba—Bai | 79.81 (5) | C4—C3—H3 | 119.4 |
O5ii—Ba—Bai | 118.14 (4) | O5—C8—O4 | 125.32 (19) |
O2W—Ba—Bai | 66.78 (4) | O5—C8—C7 | 116.23 (17) |
O1W—Ba—Bai | 75.19 (5) | O4—C8—C7 | 118.40 (17) |
O4W—Ba—Bai | 137.17 (4) | C4—C5—N1 | 121.72 (18) |
O3W—Ba—Bai | 103.23 (5) | C4—C5—H5 | 119.1 |
O2—Ba—Bai | 35.68 (3) | N1—C5—H5 | 119.1 |
O2i—Ba—O1—C6 | 12.49 (15) | O5W—Ba—C6—O1 | 36.77 (14) |
O5W—Ba—O1—C6 | −143.41 (14) | O5ii—Ba—C6—O1 | −83.81 (16) |
O5ii—Ba—O1—C6 | 126.30 (13) | O2W—Ba—C6—O1 | −100.86 (14) |
O2W—Ba—O1—C6 | 72.47 (14) | O1W—Ba—C6—O1 | 101.56 (14) |
O1W—Ba—O1—C6 | −72.75 (14) | O4W—Ba—C6—O1 | −28.14 (14) |
O4W—Ba—O1—C6 | 150.51 (15) | O3W—Ba—C6—O1 | 109.20 (15) |
O3W—Ba—O1—C6 | −94.44 (15) | O2—Ba—C6—O1 | 170.0 (2) |
O2—Ba—O1—C6 | −5.47 (12) | Bai—Ba—C6—O1 | −175.26 (15) |
Bai—Ba—O1—C6 | 4.06 (13) | O2i—Ba—C6—C4 | −102.6 (7) |
O2i—Ba—O2—C6 | −158.39 (15) | O5W—Ba—C6—C4 | 103.2 (7) |
O5W—Ba—O2—C6 | 52.26 (13) | O1—Ba—C6—C4 | 66.4 (7) |
O1—Ba—O2—C6 | 5.39 (12) | O5ii—Ba—C6—C4 | −17.4 (7) |
O5ii—Ba—O2—C6 | −111.73 (13) | O2W—Ba—C6—C4 | −34.5 (7) |
O2W—Ba—O2—C6 | −82.90 (12) | O1W—Ba—C6—C4 | 167.9 (7) |
O1W—Ba—O2—C6 | 103.21 (13) | O4W—Ba—C6—C4 | 38.3 (7) |
O4W—Ba—O2—C6 | −19.94 (13) | O3W—Ba—C6—C4 | 175.6 (7) |
O3W—Ba—O2—C6 | 133.67 (12) | O2—Ba—C6—C4 | −123.6 (7) |
Bai—Ba—O2—C6 | −158.39 (15) | Bai—Ba—C6—C4 | −108.9 (7) |
O2i—Ba—O2—Bai | 0.0 | C5—N1—C1—O3 | 174.46 (19) |
O5W—Ba—O2—Bai | −149.35 (5) | C7—N1—C1—O3 | −4.3 (3) |
O1—Ba—O2—Bai | 163.78 (9) | C5—N1—C1—C2 | −5.9 (3) |
O5ii—Ba—O2—Bai | 46.66 (10) | C7—N1—C1—C2 | 175.29 (17) |
O2W—Ba—O2—Bai | 75.49 (6) | C5—N1—C7—C8 | −95.9 (2) |
O1W—Ba—O2—Bai | −98.40 (6) | C1—N1—C7—C8 | 82.9 (2) |
O4W—Ba—O2—Bai | 138.45 (6) | O2—C6—C4—C5 | 15.6 (3) |
O3W—Ba—O2—Bai | −67.94 (7) | O1—C6—C4—C5 | −164.69 (19) |
C6—Ba—O2—Bai | 158.39 (15) | Ba—C6—C4—C5 | 134.7 (6) |
Bai—O2—C6—O1 | −136.1 (2) | O2—C6—C4—C3 | −164.05 (19) |
Ba—O2—C6—O1 | −10.0 (2) | O1—C6—C4—C3 | 15.7 (3) |
Bai—O2—C6—C4 | 43.6 (4) | Ba—C6—C4—C3 | −45.0 (8) |
Ba—O2—C6—C4 | 169.66 (16) | O3—C1—C2—C3 | −176.6 (2) |
Bai—O2—C6—Ba | −126.1 (3) | N1—C1—C2—C3 | 3.8 (3) |
Ba—O1—C6—O2 | 11.0 (2) | C1—C2—C3—C4 | 0.3 (3) |
Ba—O1—C6—C4 | −168.71 (15) | C5—C4—C3—C2 | −2.5 (3) |
O2i—Ba—C6—O2 | 21.03 (14) | C6—C4—C3—C2 | 177.12 (19) |
O5W—Ba—C6—O2 | −133.21 (12) | Baiii—O5—C8—O4 | −157.84 (15) |
O1—Ba—C6—O2 | −170.0 (2) | Baiii—O5—C8—C7 | 24.9 (3) |
O5ii—Ba—C6—O2 | 106.21 (13) | N1—C7—C8—O5 | −163.47 (17) |
O2W—Ba—C6—O2 | 89.16 (12) | N1—C7—C8—O4 | 19.0 (3) |
O1W—Ba—C6—O2 | −68.42 (12) | C3—C4—C5—N1 | 0.5 (3) |
O4W—Ba—C6—O2 | 161.88 (12) | C6—C4—C5—N1 | −179.13 (17) |
O3W—Ba—C6—O2 | −60.78 (14) | C1—N1—C5—C4 | 3.9 (3) |
Bai—Ba—C6—O2 | 14.77 (10) | C7—N1—C5—C4 | −177.34 (18) |
O2i—Ba—C6—O1 | −168.99 (14) |
Symmetry codes: (i) −x+1, −y+1, −z+1; (ii) x+1, y+1, z+1; (iii) x−1, y−1, z−1. |
D—H···A | D—H | H···A | D···A | D—H···A |
O1W—H1WA···O5iv | 0.86 (2) | 2.02 (2) | 2.863 (2) | 169 (2) |
O1W—H1WB···O2Wv | 0.84 (2) | 1.99 (2) | 2.796 (2) | 160 (2) |
O2W—H2WA···O3vi | 0.80 (2) | 1.90 (2) | 2.698 (2) | 176 (3) |
O2W—H2WB···O1Wi | 0.83 (2) | 2.03 (2) | 2.822 (2) | 162 (3) |
O3W—H3WA···O4i | 0.82 (2) | 2.02 (2) | 2.829 (3) | 174 (3) |
O3W—H3WB···O4iv | 0.85 (2) | 2.06 (2) | 2.893 (2) | 167 (3) |
O4W—H4WA···O4Wvii | 0.79 (2) | 2.17 (2) | 2.903 (4) | 156 (3) |
O4W—H4WB···O3ii | 0.79 (2) | 2.51 (3) | 2.992 (3) | 120 (2) |
O4W—H4WB···O1viii | 0.79 (2) | 2.61 (2) | 3.310 (3) | 149 (3) |
O5W—H5WA···O1viii | 0.83 (2) | 1.87 (2) | 2.689 (2) | 172 (3) |
O5W—H5WB···O4iv | 0.81 (2) | 2.02 (2) | 2.823 (3) | 171 (3) |
Symmetry codes: (i) −x+1, −y+1, −z+1; (ii) x+1, y+1, z+1; (iv) x, y+1, z+1; (v) x−1, y, z; (vi) −x+1, −y+1, −z; (vii) −x+2, −y+2, −z+1; (viii) −x+1, −y+2, −z+1. |
Experimental details
Crystal data | |
Chemical formula | [Ba(C8H5NO5)(H2O)5] |
Mr | 422.55 |
Crystal system, space group | Triclinic, P1 |
Temperature (K) | 296 |
a, b, c (Å) | 7.0051 (14), 9.7371 (19), 11.201 (2) |
α, β, γ (°) | 112.88 (3), 95.63 (3), 100.18 (3) |
V (Å3) | 681.0 (2) |
Z | 2 |
Radiation type | Mo Kα |
µ (mm−1) | 2.97 |
Crystal size (mm) | 0.16 × 0.14 × 0.10 |
Data collection | |
Diffractometer | Bruker APEXII area-detector diffractometer |
Absorption correction | Empirical (using intensity measurements) (SADABS; Sheldrick, 1996) |
Tmin, Tmax | 0.628, 0.813 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 11353, 3104, 2971 |
Rint | 0.023 |
(sin θ/λ)max (Å−1) | 0.649 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.016, 0.042, 1.01 |
No. of reflections | 3104 |
No. of parameters | 211 |
No. of restraints | 15 |
H-atom treatment | H atoms treated by a mixture of independent and constrained refinement |
Δρmax, Δρmin (e Å−3) | 0.58, −0.45 |
Computer programs: APEX2 (Bruker, 2004), SAINT (Bruker, 2004), SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), SHELXTL (Bruker, 2002).
Ba—O2i | 2.7132 (15) | Ba—O1W | 2.8560 (17) |
Ba—O5W | 2.7609 (19) | Ba—O4W | 2.856 (2) |
Ba—O1 | 2.7673 (17) | Ba—O3W | 2.8593 (19) |
Ba—O5ii | 2.8129 (19) | Ba—O2 | 2.976 (2) |
Ba—O2W | 2.8424 (18) | ||
O2i—Ba—O5ii | 81.75 (5) | O2i—Ba—O4W | 139.77 (5) |
O1—Ba—O2W | 75.98 (6) | O1—Ba—O3W | 137.63 (6) |
O5W—Ba—O1W | 69.51 (6) | O2W—Ba—O3W | 144.67 (5) |
Symmetry codes: (i) −x+1, −y+1, −z+1; (ii) x+1, y+1, z+1. |
D—H···A | D—H | H···A | D···A | D—H···A |
O1W—H1WA···O5iii | 0.855 (16) | 2.019 (18) | 2.863 (2) | 169 (2) |
O1W—H1WB···O2Wiv | 0.844 (16) | 1.988 (19) | 2.796 (2) | 160 (2) |
O2W—H2WA···O3v | 0.804 (16) | 1.897 (16) | 2.698 (2) | 176 (3) |
O2W—H2WB···O1Wi | 0.826 (16) | 2.026 (17) | 2.822 (2) | 162 (3) |
O3W—H3WA···O4i | 0.818 (17) | 2.015 (18) | 2.829 (3) | 174 (3) |
O3W—H3WB···O4iii | 0.852 (17) | 2.056 (18) | 2.893 (2) | 167 (3) |
O4W—H4WA···O4Wvi | 0.787 (16) | 2.166 (19) | 2.903 (4) | 156 (3) |
O4W—H4WB···O3ii | 0.793 (16) | 2.51 (3) | 2.992 (3) | 120 (2) |
O4W—H4WB···O1vii | 0.793 (16) | 2.608 (19) | 3.310 (3) | 149 (3) |
O5W—H5WA···O1vii | 0.831 (17) | 1.865 (17) | 2.689 (2) | 172 (3) |
O5W—H5WB···O4iii | 0.812 (17) | 2.018 (17) | 2.823 (3) | 171 (3) |
Symmetry codes: (i) −x+1, −y+1, −z+1; (ii) x+1, y+1, z+1; (iii) x, y+1, z+1; (iv) x−1, y, z; (v) −x+1, −y+1, −z; (vi) −x+2, −y+2, −z+1; (vii) −x+1, −y+2, −z+1. |
Subscribe to Acta Crystallographica Section E: Crystallographic Communications
The full text of this article is available to subscribers to the journal.
- Information on subscribing
- Sample issue
- If you have already subscribed, you may need to register
5-Carboxyl-1-carboxymethyl-2-oxidopyridinium, as a dicarboxylic acid analogue of betaine (He & Feng, 2007), own versatile coordination behavior to metal ions according to the reported complexes, [Cu(ppbet)4Cl2](ClO4)2]n (Chen et al., 1998), and [Cu(4-OPA)2]n (Zhang et al., 2006). As illustrated in Fig.1, the title complex has a binuclear structure in which the center Ba2+ is nine-coordinated by five water molecules and three carboxylic groups from three different CCOP ligands in monodentate and chelate-bridging bidentate modes, forming a tricapped trigonal prism configuration as [Ba(5—OH-BDC)(H2O)3] (Shuai et al., 2007). It is interesting that two O atoms of formate groups combine the two Ba2+ to form a rhombus while two CCOP ligands adopting the opposite orientations act as bridges to join these rhombuses to be a one-dimensional double chain. It is worth to note intermolecular O—H···O hydrogen bonds are formed to link neighboring chains to form a three-dimensional network. Besides, strong offset face-to-face π-π interactions between pyridinum groups are also involved with the plane-to-plane distance of 3.306 (1) Å and the centroid-centroid distance of 3.424 (3) Å (Fig.2).