Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807041657/bx2104sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536807041657/bx2104Isup2.hkl |
CCDC reference: 1140996
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (C-C) = 0.009 Å
- R factor = 0.038
- wR factor = 0.122
- Data-to-parameter ratio = 11.2
checkCIF/PLATON results
No syntax errors found
Alert level B PLAT027_ALERT_3_B _diffrn_reflns_theta_full (too) Low ............ 24.97 Deg. PLAT417_ALERT_2_B Short Inter D-H..H-D H2 .. H5W .. 1.90 Ang. PLAT420_ALERT_2_B D-H Without Acceptor O10 - H4W ... ? PLAT420_ALERT_2_B D-H Without Acceptor O11 - H5W ... ?
Alert level C PLAT062_ALERT_4_C Rescale T(min) & T(max) by ..................... 0.84 PLAT220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 3.33 Ratio PLAT220_ALERT_2_C Large Non-Solvent O Ueq(max)/Ueq(min) ... 2.87 Ratio PLAT222_ALERT_3_C Large Non-Solvent H Ueq(max)/Ueq(min) ... 3.81 Ratio PLAT342_ALERT_3_C Low Bond Precision on C-C Bonds (x 1000) Ang ... 9 PLAT417_ALERT_2_C Short Inter D-H..H-D H4W .. H12W .. 2.12 Ang. PLAT480_ALERT_4_C Long H...A H-Bond Reported H3W .. O12 .. 2.85 Ang. PLAT480_ALERT_4_C Long H...A H-Bond Reported H4W .. O11 .. 2.68 Ang. PLAT482_ALERT_4_C Small D-H..A Angle Rep for O10 .. O11 .. 90.00 Deg. PLAT756_ALERT_4_C H...A Calc 1.70000, Rep 1.700(10) ...... Senseless su H2 -O11 1.555 1.555
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 0.837 Tmax scaled 0.355 Tmin scaled 0.296 PLAT199_ALERT_1_G Check the Reported _cell_measurement_temperature 293 K PLAT200_ALERT_1_G Check the Reported _diffrn_ambient_temperature . 293 K PLAT794_ALERT_5_G Check Predicted Bond Valency for Ho1 (3) 1.88 PLAT860_ALERT_3_G Note: Number of Least-Squares Restraints ....... 18
0 ALERT level A = In general: serious problem 4 ALERT level B = Potentially serious problem 10 ALERT level C = Check and explain 5 ALERT level G = General alerts; check 2 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 6 ALERT type 2 Indicator that the structure model may be wrong or deficient 5 ALERT type 3 Indicator that the structure quality may be low 5 ALERT type 4 Improvement, methodology, query or suggestion 1 ALERT type 5 Informative message, check
For related literature, see: Li et al. (1993); Gao et al. (2004); Go et al. (2004); An et al. (2000); Baroni et al. (1996); Hundal et al. (2002). Isostructural lanthanide compounds have been reported with LaIII (Guerriero et al., 1987; Ghosh & Bharadwaj, 2005), CeIII (Okabe et al., 2002; Ghosh & Bharadwaj, 2003; Rafizadeh et al., 2005; Ramezanipour et al., 2005), PrIII (Ghosh & Bharadwaj, 2003; Zhao et al., 2005), NdIII (Miao et al., 1992), SmIII (Liu et al., 2005, 2006; Rafizadeh et al., 2005; Song et al., 2005), EuIII (Brayshaw et al., 2005), GdIII (Hao & Yu, 2007a) and TbIII (Hao & Yu, 2007b).
A mixture of Holmium oxide (0.1 mmol, 0.38 g), pyridine-2,6-dicarboxylic acid (0.2 mmol, 0.33 g), H2O (16 ml) in a 25 ml Teflon-lined stainless steel autoclave was kept at 473 K for three days. Colorless crystals were obtained after cooling to room temperature with a yield of 6%. Anal. Calc. for C14H19HoN2O14: C 28.43, H 3.21, N 4.74%; Found: C 28.38, H 3.23, N 4.71%.
The H atoms of the water molecule were located from difference density maps and were refined with distance restraints of d(H—H) = 1.38 (2) Å and d(O—H) = 0.82 (2) Å. All other H atoms were placed in calculated positions with a C—H bond distance of 0.93%A and Uiso(H) = 1.2Ueq of the respective carrier atom.
Complexes containing carboxyl acids have been the interest of chemists these years due to their potential applications, such as catalysis, optics, information storage, medicine, molecular electrochemistry, biochemistry and biological pharmaceutics (Li et al. (1993); Gao et al. (2004); Go et al. (2004)) Thus far, N-containing aromatic carboxyl acid has been widely used in dye intermediate, organic synthesis, sensitization material, functional pigment, adipiodone and acetrizoic acid (An et al. (2000). Pyridine carboxylic acid is also a good ligand in coordination chemistry due to its strong coordination ability and versatile coordination modes, so much attention has been paid to it in these decades (Baroni et al. (1996); Hundal et al. (2002)). Herein, we report the new complex, catena-Poly[[[diaqua(6-carboxypyridine-2-carboxylato)Holmium(III)]- µ-pyridine-2,6-dicarboxylato] tetrahydrate].
In the title compound, HoIII is of nona-coordination, chelated by two independent 2, 6-pyridine dicarboxylate, and further coordinated by two water molecules (Fig. 1). The unit is linked by one carboxylate oxygen of neighboring 2, 6-pyridine dicarboxylate forming infinite chains (Fig. 2). Extensive hydrogen bonding (Table 2) via hydrogen bonds between carboxylate oxygen atoms of 2,6-pyridinedicarboxylate and lattice water molecules or coordinated aqua ligands gives rise to three dimensional network (Fig. 3).
For related literature, see: Li et al. (1993); Gao et al. (2004); Go et al. (2004); An et al. (2000); Baroni et al. (1996); Hundal et al. (2002). Isostructural lanthanide compounds have been reported with LaIII (Guerriero et al., 1987; Ghosh & Bharadwaj, 2005), CeIII (Okabe et al., 2002; Ghosh & Bharadwaj, 2003; Rafizadeh et al., 2005; Ramezanipour et al., 2005), PrIII (Ghosh & Bharadwaj, 2003; Zhao et al., 2005), NdIII (Miao et al., 1992), SmIII (Liu et al., 2005, 2006; Rafizadeh et al., 2005; Song et al., 2005), EuIII (Brayshaw et al., 2005), GdIII (Hao & Yu, 2007a) and TbIII (Hao & Yu, 2007b).
Data collection: APEX2 (Bruker, 2004); cell refinement: SAINT-Plus (Bruker, 2001); data reduction: SAINT-Plus (Bruker, 2001); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Bruker, 2001); software used to prepare material for publication: SHELXTL (Bruker, 2001).
[Ho(C7H3NO4)(C7H4NO4)(H2O)2]·4H2O | F(000) = 1184 |
Mr = 604.24 | Dx = 1.979 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ybc | Cell parameters from 3546 reflections |
a = 14.1227 (5) Å | θ = 2.3–25.0° |
b = 11.2565 (4) Å | µ = 3.98 mm−1 |
c = 13.0342 (5) Å | T = 293 K |
β = 101.892 (1)° | Block, colorless |
V = 2027.60 (13) Å3 | 0.33 × 0.30 × 0.26 mm |
Z = 4 |
Bruker APEX II CCD area-detector diffractometer | 3546 independent reflections |
Radiation source: fine-focus sealed tube | 3213 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.022 |
φ and ω scans | θmax = 25.0°, θmin = 2.3° |
Absorption correction: multi-scan (SADABS; Bruker, 2001) | h = −16→16 |
Tmin = 0.354, Tmax = 0.424 | k = −13→13 |
7113 measured reflections | l = −7→15 |
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)] = 0.038 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.122 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.00 | w = 1/[σ2(Fo2) + (0.098P)2 + 5.4784P] where P = (Fo2 + 2Fc2)/3 |
3546 reflections | (Δ/σ)max < 0.001 |
317 parameters | Δρmax = 1.28 e Å−3 |
18 restraints | Δρmin = −1.07 e Å−3 |
[Ho(C7H3NO4)(C7H4NO4)(H2O)2]·4H2O | V = 2027.60 (13) Å3 |
Mr = 604.24 | Z = 4 |
Monoclinic, P21/c | Mo Kα radiation |
a = 14.1227 (5) Å | µ = 3.98 mm−1 |
b = 11.2565 (4) Å | T = 293 K |
c = 13.0342 (5) Å | 0.33 × 0.30 × 0.26 mm |
β = 101.892 (1)° |
Bruker APEX II CCD area-detector diffractometer | 3546 independent reflections |
Absorption correction: multi-scan (SADABS; Bruker, 2001) | 3213 reflections with I > 2σ(I) |
Tmin = 0.354, Tmax = 0.424 | Rint = 0.022 |
7113 measured reflections |
R[F2 > 2σ(F2)] = 0.038 | 18 restraints |
wR(F2) = 0.122 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.00 | Δρmax = 1.28 e Å−3 |
3546 reflections | Δρmin = −1.07 e Å−3 |
317 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 | ||
C1 | 0.4422 (5) | 0.4997 (5) | 0.6323 (5) | 0.0266 (13) | |
C2 | 0.4323 (4) | 0.0766 (5) | 0.6274 (5) | 0.0218 (12) | |
C3 | 0.2257 (4) | 0.3472 (4) | 0.3809 (4) | 0.0139 (10) | |
C4 | 0.1196 (4) | 0.5249 (5) | 0.6731 (4) | 0.0167 (11) | |
C5 | 0.5032 (5) | 0.3901 (6) | 0.6334 (5) | 0.0279 (13) | |
C6 | 0.6008 (5) | 0.3890 (8) | 0.6347 (7) | 0.0314 (8) | |
H6 | 0.6346 | 0.4600 | 0.6351 | 0.058* | |
C7 | 0.6479 (7) | 0.2832 (8) | 0.6354 (10) | 0.0366 (11) | |
H7 | 0.7144 | 0.2811 | 0.6389 | 0.076* | |
C8 | 0.5951 (6) | 0.1783 (8) | 0.6309 (8) | 0.0378 (11) | |
H8 | 0.6251 | 0.1050 | 0.6285 | 0.060* | |
C9 | 0.4969 (5) | 0.1852 (6) | 0.6301 (5) | 0.0245 (13) | |
C10 | 0.1738 (3) | 0.4516 (4) | 0.4171 (4) | 0.0121 (10) | |
C11 | 0.1380 (4) | 0.5471 (5) | 0.3507 (4) | 0.0174 (11) | |
H11 | 0.1413 | 0.5467 | 0.2801 | 0.021* | |
C12 | 0.0980 (4) | 0.6409 (5) | 0.3942 (4) | 0.0223 (12) | |
H12 | 0.0750 | 0.7063 | 0.3530 | 0.027* | |
C13 | 0.0916 (4) | 0.6390 (5) | 0.4995 (4) | 0.0206 (11) | |
H13 | 0.0648 | 0.7026 | 0.5292 | 0.025* | |
C14 | 0.1266 (3) | 0.5392 (4) | 0.5595 (4) | 0.0112 (9) | |
Ho1 | 0.269861 (18) | 0.29481 (2) | 0.648479 (18) | 0.01835 (15) | |
H1W | 0.020 (8) | 0.259 (4) | 0.338 (7) | 0.080* | |
H2W | 0.066 (7) | 0.163 (8) | 0.305 (5) | 0.080* | |
H3W | 0.216 (8) | 0.960 (5) | 0.619 (6) | 0.080* | |
H4W | 0.220 (9) | 0.900 (8) | 0.528 (5) | 0.080* | |
H5W | 0.330 (5) | 0.729 (8) | 0.608 (8) | 0.080* | |
H6W | 0.378 (7) | 0.820 (8) | 0.569 (6) | 0.080* | |
H7W | 0.135 (8) | 0.192 (8) | 0.505 (3) | 0.080* | |
H8W | 0.088 (6) | 0.131 (7) | 0.572 (7) | 0.080* | |
H9W | 0.418 (3) | 0.315 (9) | 0.852 (7) | 0.080* | |
H10W | 0.326 (5) | 0.342 (10) | 0.863 (6) | 0.080* | |
H11W | 0.025 (6) | 0.4863 (18) | 0.891 (8) | 0.080* | |
H12W | 0.083 (3) | 0.584 (7) | 0.926 (8) | 0.080* | |
N1 | 0.1688 (3) | 0.4484 (3) | 0.5189 (3) | 0.0102 (8) | |
N2 | 0.4520 (4) | 0.2880 (4) | 0.6325 (4) | 0.0196 (11) | |
O1 | 0.3567 (3) | 0.4920 (3) | 0.6354 (3) | 0.0243 (9) | |
O2 | 0.4875 (4) | 0.6000 (4) | 0.6264 (5) | 0.0454 (13) | |
H2 | 0.4537 | 0.6554 | 0.6384 | 0.068* | |
O3 | 0.4692 (3) | −0.0218 (4) | 0.6230 (4) | 0.0385 (12) | |
O4 | 0.3442 (3) | 0.0968 (3) | 0.6298 (3) | 0.0215 (8) | |
O5 | 0.2737 (3) | 0.2818 (3) | 0.4533 (3) | 0.0158 (8) | |
O6 | 0.2188 (3) | 0.3335 (3) | 0.2838 (3) | 0.0182 (8) | |
O7 | 0.1549 (3) | 0.4294 (3) | 0.7180 (3) | 0.0209 (8) | |
O8 | 0.0792 (3) | 0.6042 (4) | 0.7147 (3) | 0.0291 (10) | |
O9 | 0.0416 (3) | 0.1919 (4) | 0.3505 (3) | 0.0238 (9) | |
O10 | 0.2016 (6) | 0.9006 (6) | 0.5839 (7) | 0.083 (2) | |
O11 | 0.3770 (6) | 0.7738 (6) | 0.6176 (8) | 0.086 (3) | |
O12 | 0.1248 (3) | 0.1839 (4) | 0.5634 (3) | 0.0250 (9) | |
O13 | 0.3662 (4) | 0.3461 (5) | 0.8260 (3) | 0.0356 (11) | |
O14 | 0.0295 (3) | 0.5577 (4) | 0.9011 (4) | 0.0317 (10) |
U11 | U22 | U33 | U12 | U13 | U23 | |
C1 | 0.035 (4) | 0.017 (3) | 0.026 (3) | −0.008 (2) | 0.001 (3) | 0.002 (2) |
C2 | 0.013 (3) | 0.028 (3) | 0.024 (3) | −0.001 (2) | 0.001 (2) | 0.000 (2) |
C3 | 0.016 (3) | 0.014 (2) | 0.013 (2) | 0.003 (2) | 0.0043 (19) | 0.000 (2) |
C4 | 0.016 (3) | 0.018 (3) | 0.017 (3) | 0.001 (2) | 0.004 (2) | −0.001 (2) |
C5 | 0.026 (3) | 0.028 (3) | 0.030 (3) | −0.013 (3) | 0.006 (2) | 0.002 (3) |
C6 | 0.0177 (15) | 0.0427 (19) | 0.0322 (19) | 0.002 (2) | −0.0009 (13) | 0.000 (2) |
C7 | 0.026 (2) | 0.050 (3) | 0.033 (3) | 0.005 (2) | 0.0015 (19) | −0.001 (2) |
C8 | 0.031 (2) | 0.043 (2) | 0.038 (3) | 0.003 (2) | 0.0025 (19) | 0.003 (2) |
C9 | 0.015 (3) | 0.028 (3) | 0.030 (3) | −0.003 (2) | 0.002 (2) | 0.001 (2) |
C10 | 0.013 (2) | 0.013 (2) | 0.009 (2) | −0.0024 (19) | 0.0009 (18) | −0.0014 (18) |
C11 | 0.025 (3) | 0.017 (3) | 0.009 (2) | 0.007 (2) | 0.001 (2) | 0.0026 (19) |
C12 | 0.032 (3) | 0.018 (3) | 0.014 (3) | 0.009 (2) | −0.002 (2) | 0.005 (2) |
C13 | 0.027 (3) | 0.016 (3) | 0.020 (3) | 0.007 (2) | 0.007 (2) | 0.001 (2) |
C14 | 0.013 (2) | 0.009 (2) | 0.012 (2) | 0.0019 (18) | 0.0023 (18) | −0.0009 (18) |
Ho1 | 0.0194 (2) | 0.0194 (2) | 0.0157 (2) | 0.00111 (8) | 0.00213 (13) | 0.00128 (8) |
N1 | 0.011 (2) | 0.0103 (19) | 0.0092 (19) | 0.0014 (15) | 0.0026 (15) | 0.0016 (15) |
N2 | 0.016 (3) | 0.026 (3) | 0.016 (2) | 0.0007 (18) | 0.001 (2) | −0.0005 (17) |
O1 | 0.024 (2) | 0.0156 (19) | 0.031 (2) | −0.0079 (16) | 0.0020 (17) | 0.0028 (16) |
O2 | 0.047 (3) | 0.026 (2) | 0.062 (3) | −0.015 (2) | 0.009 (3) | 0.004 (2) |
O3 | 0.028 (2) | 0.019 (2) | 0.065 (3) | 0.0107 (19) | 0.002 (2) | −0.002 (2) |
O4 | 0.020 (2) | 0.0129 (18) | 0.031 (2) | 0.0005 (15) | 0.0038 (16) | 0.0016 (15) |
O5 | 0.020 (2) | 0.0185 (18) | 0.0081 (17) | 0.0112 (14) | 0.0008 (15) | 0.0013 (13) |
O6 | 0.026 (2) | 0.0183 (18) | 0.0084 (18) | 0.0066 (16) | −0.0004 (15) | −0.0025 (15) |
O7 | 0.033 (2) | 0.0191 (19) | 0.0123 (17) | 0.0125 (16) | 0.0085 (16) | 0.0044 (14) |
O8 | 0.049 (3) | 0.020 (2) | 0.023 (2) | 0.0165 (19) | 0.0192 (19) | 0.0009 (16) |
O9 | 0.024 (2) | 0.028 (2) | 0.019 (2) | 0.0023 (16) | 0.0023 (18) | −0.0009 (16) |
O10 | 0.065 (5) | 0.035 (3) | 0.132 (7) | −0.013 (3) | −0.017 (5) | 0.001 (4) |
O11 | 0.066 (5) | 0.035 (3) | 0.152 (8) | −0.004 (3) | 0.013 (5) | 0.012 (4) |
O12 | 0.028 (2) | 0.035 (2) | 0.0105 (19) | −0.0128 (18) | 0.0000 (17) | 0.0046 (16) |
O13 | 0.037 (3) | 0.054 (3) | 0.014 (2) | −0.029 (2) | −0.0008 (18) | 0.000 (2) |
O14 | 0.040 (3) | 0.030 (2) | 0.030 (2) | 0.011 (2) | 0.019 (2) | −0.0005 (19) |
C1—O1 | 1.219 (8) | C13—C14 | 1.399 (7) |
C1—O2 | 1.307 (8) | C13—H13 | 0.9300 |
C1—C5 | 1.503 (9) | C14—N1 | 1.345 (6) |
C2—O3 | 1.231 (7) | Ho1—O12 | 2.460 (4) |
C2—O4 | 1.271 (7) | Ho1—O4 | 2.497 (4) |
C2—C9 | 1.521 (8) | Ho1—O6i | 2.499 (4) |
C3—O6 | 1.259 (6) | Ho1—O13 | 2.499 (4) |
C3—O5 | 1.276 (6) | Ho1—O7 | 2.522 (4) |
C3—C10 | 1.511 (7) | Ho1—O1 | 2.559 (4) |
C4—O8 | 1.241 (7) | Ho1—O5 | 2.559 (4) |
C4—O7 | 1.275 (6) | Ho1—N2 | 2.625 (5) |
C4—C14 | 1.514 (7) | Ho1—N1 | 2.623 (4) |
C5—N2 | 1.357 (7) | O2—H2 | 0.8200 |
C5—C6 | 1.376 (10) | O6—Ho1ii | 2.499 (4) |
C6—C7 | 1.364 (12) | O9—H1W | 0.82 (5) |
C6—H6 | 0.9300 | O9—H2W | 0.81 (8) |
C7—C8 | 1.391 (12) | O10—H3W | 0.81 (7) |
C7—H7 | 0.9300 | O10—H4W | 0.82 (9) |
C8—C9 | 1.387 (10) | O11—H5W | 0.82 (8) |
C8—H8 | 0.9300 | O11—H6W | 0.82 (9) |
C9—N2 | 1.323 (8) | O12—H7W | 0.81 (6) |
C10—N1 | 1.345 (6) | O12—H8W | 0.81 (8) |
C10—C11 | 1.407 (7) | O13—H9W | 0.82 (7) |
C11—C12 | 1.374 (8) | O13—H10W | 0.82 (7) |
C11—H11 | 0.9300 | O14—H11W | 0.815 (11) |
C12—C13 | 1.395 (8) | O14—H12W | 0.81 (7) |
C12—H12 | 0.9300 | ||
O1—C1—O2 | 124.3 (6) | O6i—Ho1—O7 | 78.04 (12) |
O1—C1—C5 | 120.7 (5) | O13—Ho1—O7 | 78.27 (16) |
O2—C1—C5 | 115.0 (6) | O12—Ho1—O1 | 140.95 (13) |
O3—C2—O4 | 126.0 (6) | O4—Ho1—O1 | 123.42 (14) |
O3—C2—C9 | 117.8 (5) | O6i—Ho1—O1 | 139.51 (13) |
O4—C2—C9 | 116.2 (5) | O13—Ho1—O1 | 71.59 (14) |
O6—C3—O5 | 126.4 (5) | O7—Ho1—O1 | 81.70 (13) |
O6—C3—C10 | 117.8 (4) | O12—Ho1—O5 | 73.07 (13) |
O5—C3—C10 | 115.8 (4) | O4—Ho1—O5 | 75.91 (12) |
O8—C4—O7 | 125.3 (5) | O6i—Ho1—O5 | 137.46 (12) |
O8—C4—C14 | 118.6 (5) | O13—Ho1—O5 | 144.57 (14) |
O7—C4—C14 | 116.1 (4) | O7—Ho1—O5 | 122.56 (11) |
N2—C5—C6 | 121.5 (7) | O1—Ho1—O5 | 82.82 (13) |
N2—C5—C1 | 113.1 (5) | O12—Ho1—N2 | 133.50 (15) |
C6—C5—C1 | 125.4 (6) | O4—Ho1—N2 | 61.78 (13) |
C7—C6—C5 | 119.6 (7) | O6i—Ho1—N2 | 117.99 (14) |
C7—C6—H6 | 120.2 | O13—Ho1—N2 | 74.01 (16) |
C5—C6—H6 | 120.2 | O7—Ho1—N2 | 139.50 (14) |
C6—C7—C8 | 119.0 (8) | O1—Ho1—N2 | 61.90 (13) |
C6—C7—H7 | 120.5 | O5—Ho1—N2 | 72.42 (14) |
C8—C7—H7 | 120.5 | O12—Ho1—N1 | 75.65 (13) |
C9—C8—C7 | 118.6 (8) | O4—Ho1—N1 | 135.17 (13) |
C9—C8—H8 | 120.7 | O6i—Ho1—N1 | 129.61 (13) |
C7—C8—H8 | 120.7 | O13—Ho1—N1 | 124.34 (16) |
N2—C9—C8 | 122.2 (6) | O7—Ho1—N1 | 61.97 (11) |
N2—C9—C2 | 114.5 (5) | O1—Ho1—N1 | 65.81 (13) |
C8—C9—C2 | 123.3 (6) | O5—Ho1—N1 | 61.19 (11) |
N1—C10—C11 | 122.9 (4) | N2—Ho1—N1 | 112.35 (13) |
N1—C10—C3 | 114.5 (4) | C14—N1—C10 | 119.0 (4) |
C11—C10—C3 | 122.6 (4) | C14—N1—Ho1 | 118.3 (3) |
C12—C11—C10 | 117.3 (5) | C10—N1—Ho1 | 121.4 (3) |
C12—C11—H11 | 121.3 | C9—N2—C5 | 119.0 (6) |
C10—C11—H11 | 121.3 | C9—N2—Ho1 | 120.7 (4) |
C11—C12—C13 | 120.7 (5) | C5—N2—Ho1 | 120.2 (4) |
C11—C12—H12 | 119.6 | C1—O1—Ho1 | 123.7 (4) |
C13—C12—H12 | 119.7 | C1—O2—H2 | 109.5 |
C12—C13—C14 | 118.4 (5) | C2—O4—Ho1 | 126.6 (4) |
C12—C13—H13 | 120.8 | C3—O5—Ho1 | 125.9 (3) |
C14—C13—H13 | 120.8 | C3—O6—Ho1ii | 143.8 (3) |
N1—C14—C13 | 121.7 (4) | C4—O7—Ho1 | 124.2 (3) |
N1—C14—C4 | 115.3 (4) | H1W—O9—H2W | 115 (9) |
C13—C14—C4 | 123.0 (4) | H3W—O10—H4W | 115 (9) |
O12—Ho1—O4 | 80.27 (15) | H5W—O11—H6W | 114 (10) |
O12—Ho1—O6i | 71.96 (12) | Ho1—O12—H7W | 94 (7) |
O4—Ho1—O6i | 75.01 (13) | Ho1—O12—H8W | 144 (6) |
O12—Ho1—O13 | 141.17 (13) | H7W—O12—H8W | 117 (9) |
O4—Ho1—O13 | 97.86 (16) | Ho1—O13—H9W | 123 (8) |
O6i—Ho1—O13 | 70.18 (13) | Ho1—O13—H10W | 103 (7) |
O12—Ho1—O7 | 85.92 (15) | H9W—O13—H10W | 114 (8) |
O4—Ho1—O7 | 152.41 (12) | H11W—O14—H12W | 117 (8) |
Symmetry codes: (i) x, −y+1/2, z+1/2; (ii) x, −y+1/2, z−1/2. |
D—H···A | D—H | H···A | D···A | D—H···A |
O9—H1W···O8iii | 0.82 (5) | 2.10 (4) | 2.882 (6) | 160 (12) |
O9—H2W···O7ii | 0.81 (8) | 2.13 (9) | 2.924 (6) | 166 (9) |
O10—H3W···O12iv | 0.81 (7) | 2.85 (10) | 3.361 (8) | 123 (10) |
O10—H4W···O11 | 0.82 (9) | 2.68 (13) | 2.813 (11) | 90 (9) |
O11—H6W···O3iv | 0.82 (9) | 2.23 (9) | 2.638 (8) | 111 (8) |
O12—H7W···O9 | 0.81 (6) | 2.16 (7) | 2.782 (6) | 133 (10) |
O12—H8W···O14v | 0.81 (8) | 1.95 (9) | 2.720 (6) | 158 (11) |
O13—H9W···O3vi | 0.82 (7) | 2.41 (10) | 2.724 (6) | 104 (8) |
O13—H10W···O5i | 0.82 (7) | 2.06 (7) | 2.725 (5) | 139 (10) |
O14—H11W···O9i | 0.82 (1) | 2.10 (3) | 2.899 (6) | 168 (10) |
O2—H2···O11 | 0.82 (1) | 1.70 (1) | 2.491 (9) | 160 (1) |
Symmetry codes: (i) x, −y+1/2, z+1/2; (ii) x, −y+1/2, z−1/2; (iii) −x, −y+1, −z+1; (iv) x, y+1, z; (v) −x, y−1/2, −z+3/2; (vi) −x+1, y+1/2, −z+3/2. |
Experimental details
Crystal data | |
Chemical formula | [Ho(C7H3NO4)(C7H4NO4)(H2O)2]·4H2O |
Mr | 604.24 |
Crystal system, space group | Monoclinic, P21/c |
Temperature (K) | 293 |
a, b, c (Å) | 14.1227 (5), 11.2565 (4), 13.0342 (5) |
β (°) | 101.892 (1) |
V (Å3) | 2027.60 (13) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 3.98 |
Crystal size (mm) | 0.33 × 0.30 × 0.26 |
Data collection | |
Diffractometer | Bruker APEX II CCD area-detector |
Absorption correction | Multi-scan (SADABS; Bruker, 2001) |
Tmin, Tmax | 0.354, 0.424 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 7113, 3546, 3213 |
Rint | 0.022 |
(sin θ/λ)max (Å−1) | 0.594 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.038, 0.122, 1.00 |
No. of reflections | 3546 |
No. of parameters | 317 |
No. of restraints | 18 |
H-atom treatment | H atoms treated by a mixture of independent and constrained refinement |
Δρmax, Δρmin (e Å−3) | 1.28, −1.07 |
Computer programs: APEX2 (Bruker, 2004), SAINT-Plus (Bruker, 2001), SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), SHELXTL (Bruker, 2001).
D—H···A | D—H | H···A | D···A | D—H···A |
O9—H1W···O8i | 0.82 (5) | 2.10 (4) | 2.882 (6) | 160 (12) |
O9—H2W···O7ii | 0.81 (8) | 2.13 (9) | 2.924 (6) | 166 (9) |
O10—H3W···O12iii | 0.81 (7) | 2.85 (10) | 3.361 (8) | 123 (10) |
O10—H4W···O11 | 0.82 (9) | 2.68 (13) | 2.813 (11) | 90 (9) |
O11—H6W···O3iii | 0.82 (9) | 2.23 (9) | 2.638 (8) | 111 (8) |
O12—H7W···O9 | 0.81 (6) | 2.16 (7) | 2.782 (6) | 133 (10) |
O12—H8W···O14iv | 0.81 (8) | 1.95 (9) | 2.720 (6) | 158 (11) |
O13—H9W···O3v | 0.82 (7) | 2.41 (10) | 2.724 (6) | 104 (8) |
O13—H10W···O5vi | 0.82 (7) | 2.06 (7) | 2.725 (5) | 139 (10) |
O14—H11W···O9vi | 0.815 (11) | 2.10 (3) | 2.899 (6) | 168 (10) |
O2—H2···O11 | 0.82 (0) | 1.70 (1) | 2.491 (9) | 160.22 (0) |
Symmetry codes: (i) −x, −y+1, −z+1; (ii) x, −y+1/2, z−1/2; (iii) x, y+1, z; (iv) −x, y−1/2, −z+3/2; (v) −x+1, y+1/2, −z+3/2; (vi) x, −y+1/2, z+1/2. |
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Complexes containing carboxyl acids have been the interest of chemists these years due to their potential applications, such as catalysis, optics, information storage, medicine, molecular electrochemistry, biochemistry and biological pharmaceutics (Li et al. (1993); Gao et al. (2004); Go et al. (2004)) Thus far, N-containing aromatic carboxyl acid has been widely used in dye intermediate, organic synthesis, sensitization material, functional pigment, adipiodone and acetrizoic acid (An et al. (2000). Pyridine carboxylic acid is also a good ligand in coordination chemistry due to its strong coordination ability and versatile coordination modes, so much attention has been paid to it in these decades (Baroni et al. (1996); Hundal et al. (2002)). Herein, we report the new complex, catena-Poly[[[diaqua(6-carboxypyridine-2-carboxylato)Holmium(III)]- µ-pyridine-2,6-dicarboxylato] tetrahydrate].
In the title compound, HoIII is of nona-coordination, chelated by two independent 2, 6-pyridine dicarboxylate, and further coordinated by two water molecules (Fig. 1). The unit is linked by one carboxylate oxygen of neighboring 2, 6-pyridine dicarboxylate forming infinite chains (Fig. 2). Extensive hydrogen bonding (Table 2) via hydrogen bonds between carboxylate oxygen atoms of 2,6-pyridinedicarboxylate and lattice water molecules or coordinated aqua ligands gives rise to three dimensional network (Fig. 3).