Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807038846/gw2020sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536807038846/gw2020Isup2.hkl |
CCDC reference: 660105
Key indicators
- Single-crystal X-ray study
- T = 294 K
- Mean (C-C) = 0.005 Å
- R factor = 0.021
- wR factor = 0.052
- Data-to-parameter ratio = 12.4
checkCIF/PLATON results
No syntax errors found
Alert level C PLAT066_ALERT_1_C Predicted and Reported Transmissions Identical . ? PLAT125_ALERT_4_C No _symmetry_space_group_name_Hall Given ....... ? PLAT180_ALERT_3_C Check Cell Rounding: # of Values Ending with 0 = 3 PLAT222_ALERT_3_C Large Non-Solvent H Ueq(max)/Ueq(min) ... 4.00 Ratio PLAT245_ALERT_2_C U(iso) H2A Smaller than U(eq) N2 by ... 0.01 AngSq PLAT420_ALERT_2_C D-H Without Acceptor N2 - H2B ... ? PLAT420_ALERT_2_C D-H Without Acceptor N3 - H3B ... ? PLAT731_ALERT_1_C Bond Calc 0.85(3), Rep 0.849(10) ...... 3.00 su-Ra N2 -H2A 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 0.86(3), Rep 0.856(10) ...... 3.00 su-Ra N3 -H3B 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 0.82(3), Rep 0.817(10) ...... 3.00 su-Ra O7 -H7A 1.555 1.555 PLAT735_ALERT_1_C D-H Calc 0.85(3), Rep 0.849(10) ...... 3.00 su-Ra N2 -H2A 1.555 1.555 PLAT735_ALERT_1_C D-H Calc 0.82(3), Rep 0.817(10) ...... 3.00 su-Ra O7 -H7A 1.555 1.555 PLAT736_ALERT_1_C H...A Calc 2.08(4), Rep 2.079(16) ...... 2.50 su-Ra H7A -N3 1.555 2.646
Alert level G PLAT794_ALERT_5_G Check Predicted Bond Valency for Ho (3) 2.44 PLAT860_ALERT_3_G Note: Number of Least-Squares Restraints ....... 10
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 13 ALERT level C = Check and explain 2 ALERT level G = General alerts; check 7 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 3 ALERT type 2 Indicator that the structure model may be wrong or deficient 3 ALERT type 3 Indicator that the structure quality may be low 1 ALERT type 4 Improvement, methodology, query or suggestion 1 ALERT type 5 Informative message, check
For related literature, see: Chen et al. (2006); Chu et al. (2001); Kepert & Rosseinsky (1998); Reineke et al. (1999).
A mixture of Ho2O3 (0.25 mmol), 4-aminobenzonitrile (2.0 mmol), H2O (10 ml, 0.55 mmol) and two drops of acetic acid with the pH value of about 3.0, was heated in a 25 ml capacity Teflon-lined reaction vessel at 160 ° for 5 days, the reaction mixture was cooled to room temperature over a period of 48 h. The product was collected by filtration, washed with H2O and air-dried, colorless crystals suitable for X-ray analysis were obtained. Analysis calculated (%): C, 42.62; H, 3.38; N, 7.10%; Found: C, 43.05; H, 3.32%; N, 7.17%.
H atoms bonded to C atoms were placed geometrically and treated as riding, (C—H distances are 0.93 Å), with Uiso(H) = 1.2Ueq(C). The water H atoms found from Fourier difference maps were refined with restraints for O—H distances (0.816–0.817 Å) and Uiso(H) fixed at 0.05.
During the last two decades, lanthanide complexes have received much attention because of their interesting photophysical properties which have potential applications in the luminescent probes for chemical or biological macromolecules and the active center for luminescent materials(Chu et al., 2001; Kepert & Rosseinsky, 1998; Reineke et al., 1999; Chen et al., 2006;). We have chosen 4-aminobenzonitrile as ligand and investigated its reaction with Ho2O3 under hydrothermal synthesis, and report herein the X-ray crystal structure of the novel terbium coordination polymer, [Ho(4-aminobenzoate)3(H2O)]n, (I).
In (I) (Fig. 1), the HoIII center is eight-coordinated by six O atoms from five different 4-aminobenzoate ligands, one N atoms from a 4-aminobenzoate ligand and one O atoms from a coordinated water molecule, thus the HoIII ion has a distorted bicapped trigonal prism. In the coordination polyhedron of HoIII ion, the Ho—O distance of carboxyl is in the range 2.337 (2)–2.482 (2) Å, and the mean Ho—O bond length is 2.428 (2) Å. The Ho—O bond length involving the coordination water is 2.546 (2) Å, and the Ho—N distance is 2.691 (3) Å. In (I), each 4-aminobenzoate ligand adopts an O,O-bidentate bridging mode using a carboxylate group. Adjacent HoIII centers are doubly bridged by the ligands, forming a big eight-membered ring, while the other two Ho atoms has a 16-membered ring bridged by the carboxylate groups and amino groups (Fig. 2).
For related literature, see: Chen et al. (2006); Chu et al. (2001); Kepert & Rosseinsky (1998); Reineke et al. (1999).
Data collection: SMART (Bruker, 2001); cell refinement: SMART; data reduction: SAINT (Bruker, 2003); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Sheldrick, 2003); software used to prepare material for publication: SHELXTL.
[Ho(C7H6NO2)3(H2O)] | F(000) = 1160 |
Mr = 591.33 | Dx = 1.824 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
a = 9.772 (1) Å | Cell parameters from 30 reflections |
b = 22.761 (3) Å | θ = 4.9–13.5° |
c = 9.832 (1) Å | µ = 3.72 mm−1 |
β = 100.02 (1)° | T = 294 K |
V = 2153.5 (4) Å3 | Block, colorless |
Z = 4 | 0.24 × 0.20 × 0.18 mm |
Bruker SMART CCD area-detector diffractometer | 4001 independent reflections |
Radiation source: fine-focus sealed tube | 2954 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.014 |
φ and ω scans | θmax = 25.5°, θmin = 1.8° |
Absorption correction: multi-scan (SADABS; Sheldrick, 2003) | h = 0→11 |
Tmin = 0.413, Tmax = 0.512 | k = 0→27 |
4521 measured reflections | l = −11→11 |
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)] = 0.021 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.052 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.03 | w = 1/[σ2(Fo2) + (0.027P)2] where P = (Fo2 + 2Fc2)/3 |
4005 reflections | (Δ/σ)max = 0.001 |
322 parameters | Δρmax = 0.44 e Å−3 |
10 restraints | Δρmin = −0.53 e Å−3 |
[Ho(C7H6NO2)3(H2O)] | V = 2153.5 (4) Å3 |
Mr = 591.33 | Z = 4 |
Monoclinic, P21/n | Mo Kα radiation |
a = 9.772 (1) Å | µ = 3.72 mm−1 |
b = 22.761 (3) Å | T = 294 K |
c = 9.832 (1) Å | 0.24 × 0.20 × 0.18 mm |
β = 100.02 (1)° |
Bruker SMART CCD area-detector diffractometer | 4001 independent reflections |
Absorption correction: multi-scan (SADABS; Sheldrick, 2003) | 2954 reflections with I > 2σ(I) |
Tmin = 0.413, Tmax = 0.512 | Rint = 0.014 |
4521 measured reflections |
R[F2 > 2σ(F2)] = 0.021 | 10 restraints |
wR(F2) = 0.052 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.03 | Δρmax = 0.44 e Å−3 |
4005 reflections | Δρmin = −0.53 e Å−3 |
322 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 | ||
Ho | 0.481566 (14) | 0.501123 (7) | 0.758702 (13) | 0.01914 (7) | |
O1 | 0.3005 (2) | 0.52755 (10) | 0.5758 (2) | 0.0273 (5) | |
O2 | 0.3446 (2) | 0.48881 (9) | 0.3815 (2) | 0.0288 (6) | |
O3 | 0.3698 (3) | 0.54166 (10) | 0.9282 (2) | 0.0334 (6) | |
O4 | 0.3944 (3) | 0.58076 (11) | 1.1353 (2) | 0.0371 (6) | |
O5 | 0.5125 (2) | 0.60754 (10) | 0.7181 (2) | 0.0288 (5) | |
O6 | 0.6608 (2) | 0.56728 (9) | 0.8857 (2) | 0.0272 (5) | |
N1 | −0.2838 (3) | 0.57271 (13) | 0.1850 (3) | 0.0245 (6) | |
N2 | 0.1092 (4) | 0.79410 (17) | 0.7699 (5) | 0.0550 (10) | |
N3 | 0.8320 (4) | 0.83857 (14) | 0.9754 (3) | 0.0373 (8) | |
C1 | 0.0375 (3) | 0.56663 (14) | 0.4452 (3) | 0.0253 (7) | |
H1 | 0.0687 | 0.5791 | 0.5354 | 0.030* | |
C2 | −0.0937 (3) | 0.58147 (13) | 0.3808 (3) | 0.0258 (7) | |
H2 | −0.1493 | 0.6049 | 0.4263 | 0.031* | |
C3 | −0.1444 (3) | 0.56162 (14) | 0.2473 (3) | 0.0242 (7) | |
C4 | −0.0586 (3) | 0.52806 (16) | 0.1795 (3) | 0.0317 (8) | |
H4 | −0.0911 | 0.5148 | 0.0903 | 0.038* | |
C5 | 0.0748 (4) | 0.51421 (14) | 0.2436 (3) | 0.0306 (8) | |
H5 | 0.1318 | 0.4920 | 0.1971 | 0.037* | |
C6 | 0.1244 (3) | 0.53352 (14) | 0.3786 (3) | 0.0219 (7) | |
C7 | 0.2652 (3) | 0.51582 (12) | 0.4497 (3) | 0.0217 (7) | |
C8 | 0.2766 (4) | 0.68773 (15) | 1.0271 (4) | 0.0343 (8) | |
H8 | 0.3135 | 0.6867 | 1.1209 | 0.041* | |
C9 | 0.2192 (4) | 0.73920 (16) | 0.9689 (4) | 0.0401 (9) | |
H9 | 0.2185 | 0.7725 | 1.0237 | 0.048* | |
C10 | 0.1626 (4) | 0.74188 (15) | 0.8301 (4) | 0.0370 (9) | |
C11 | 0.1606 (4) | 0.69082 (16) | 0.7522 (4) | 0.0381 (9) | |
H11 | 0.1184 | 0.6912 | 0.6599 | 0.046* | |
C12 | 0.2196 (4) | 0.64017 (15) | 0.8089 (3) | 0.0339 (8) | |
H12 | 0.2193 | 0.6069 | 0.7538 | 0.041* | |
C13 | 0.2802 (3) | 0.63734 (14) | 0.9478 (3) | 0.0259 (7) | |
C14 | 0.3513 (3) | 0.58321 (14) | 1.0068 (3) | 0.0254 (7) | |
C15 | 0.8018 (4) | 0.67744 (15) | 0.9384 (3) | 0.0319 (8) | |
H15 | 0.8548 | 0.6442 | 0.9657 | 0.038* | |
C16 | 0.8547 (4) | 0.73237 (15) | 0.9764 (4) | 0.0348 (8) | |
H16 | 0.9433 | 0.7358 | 1.0286 | 0.042* | |
C17 | 0.7770 (4) | 0.78271 (14) | 0.9375 (3) | 0.0303 (8) | |
C18 | 0.6457 (4) | 0.77666 (15) | 0.8593 (4) | 0.0384 (9) | |
H18 | 0.5922 | 0.8098 | 0.8326 | 0.046* | |
C19 | 0.5935 (4) | 0.72156 (15) | 0.8207 (4) | 0.0342 (8) | |
H19 | 0.5053 | 0.7182 | 0.7676 | 0.041* | |
C20 | 0.6701 (4) | 0.67137 (14) | 0.8595 (3) | 0.0269 (7) | |
C21 | 0.6117 (3) | 0.61238 (14) | 0.8182 (3) | 0.0257 (7) | |
O7 | 0.4542 (3) | 0.41368 (11) | 0.5947 (2) | 0.0293 (5) | |
H1A | −0.292 (4) | 0.5723 (15) | 0.0963 (11) | 0.035 (10)* | |
H1B | −0.311 (3) | 0.6058 (8) | 0.210 (3) | 0.034 (10)* | |
H2A | 0.067 (3) | 0.8143 (14) | 0.822 (3) | 0.042 (12)* | |
H2B | 0.062 (4) | 0.792 (2) | 0.689 (2) | 0.12 (3)* | |
H3A | 0.888 (3) | 0.8377 (15) | 1.0532 (19) | 0.035 (11)* | |
H3B | 0.768 (3) | 0.8636 (14) | 0.981 (3) | 0.054 (14)* | |
H7A | 0.520 (3) | 0.3920 (16) | 0.590 (5) | 0.075 (17)* | |
H7B | 0.427 (4) | 0.4282 (16) | 0.519 (2) | 0.051 (13)* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Ho | 0.01833 (9) | 0.01936 (9) | 0.01852 (9) | 0.00174 (9) | −0.00016 (5) | −0.00054 (8) |
O1 | 0.0259 (12) | 0.0290 (12) | 0.0234 (12) | 0.0024 (10) | −0.0058 (10) | −0.0016 (10) |
O2 | 0.0213 (11) | 0.0363 (15) | 0.0289 (11) | 0.0033 (10) | 0.0044 (10) | −0.0005 (10) |
O3 | 0.0408 (15) | 0.0235 (12) | 0.0386 (14) | 0.0086 (11) | 0.0142 (12) | 0.0004 (11) |
O4 | 0.0403 (15) | 0.0374 (15) | 0.0291 (13) | 0.0108 (12) | −0.0063 (12) | 0.0032 (11) |
O5 | 0.0308 (13) | 0.0235 (12) | 0.0274 (12) | −0.0008 (10) | −0.0082 (11) | −0.0003 (10) |
O6 | 0.0312 (13) | 0.0218 (12) | 0.0255 (12) | 0.0006 (10) | −0.0039 (10) | 0.0026 (10) |
N1 | 0.0188 (14) | 0.0298 (16) | 0.0235 (15) | 0.0026 (12) | −0.0002 (12) | −0.0014 (13) |
N2 | 0.062 (3) | 0.038 (2) | 0.066 (3) | 0.0252 (19) | 0.013 (2) | 0.0180 (19) |
N3 | 0.041 (2) | 0.0280 (17) | 0.042 (2) | −0.0095 (15) | 0.0051 (16) | −0.0054 (14) |
C1 | 0.0233 (17) | 0.0300 (18) | 0.0205 (15) | −0.0028 (14) | −0.0013 (13) | −0.0046 (14) |
C2 | 0.0230 (17) | 0.0264 (17) | 0.0276 (17) | 0.0012 (14) | 0.0036 (14) | −0.0059 (14) |
C3 | 0.0189 (16) | 0.0293 (17) | 0.0231 (16) | 0.0003 (14) | 0.0002 (13) | 0.0047 (13) |
C4 | 0.0234 (18) | 0.048 (2) | 0.0216 (16) | 0.0016 (17) | −0.0027 (14) | −0.0081 (16) |
C5 | 0.0239 (17) | 0.044 (2) | 0.0245 (17) | 0.0034 (15) | 0.0051 (13) | −0.0073 (14) |
C6 | 0.0180 (16) | 0.0244 (17) | 0.0220 (16) | 0.0001 (13) | −0.0001 (13) | 0.0035 (13) |
C7 | 0.0189 (16) | 0.0184 (17) | 0.0272 (16) | −0.0038 (12) | 0.0024 (14) | 0.0018 (12) |
C8 | 0.032 (2) | 0.036 (2) | 0.0332 (19) | 0.0071 (17) | 0.0021 (16) | −0.0032 (16) |
C9 | 0.045 (2) | 0.0256 (19) | 0.049 (2) | 0.0056 (17) | 0.0083 (19) | −0.0072 (17) |
C10 | 0.034 (2) | 0.0284 (19) | 0.051 (2) | 0.0120 (16) | 0.0146 (18) | 0.0098 (17) |
C11 | 0.044 (2) | 0.042 (2) | 0.0256 (18) | 0.0127 (18) | −0.0008 (16) | 0.0069 (16) |
C12 | 0.041 (2) | 0.0314 (19) | 0.0285 (18) | 0.0109 (17) | 0.0032 (16) | −0.0027 (15) |
C13 | 0.0273 (18) | 0.0241 (17) | 0.0261 (17) | 0.0083 (14) | 0.0046 (14) | 0.0022 (14) |
C14 | 0.0210 (17) | 0.0245 (17) | 0.0312 (19) | 0.0039 (14) | 0.0061 (14) | 0.0043 (14) |
C15 | 0.0280 (19) | 0.0264 (18) | 0.039 (2) | −0.0015 (15) | −0.0017 (16) | 0.0009 (16) |
C16 | 0.0270 (19) | 0.036 (2) | 0.039 (2) | −0.0074 (16) | −0.0015 (16) | −0.0034 (17) |
C17 | 0.037 (2) | 0.0258 (18) | 0.0297 (18) | −0.0115 (15) | 0.0109 (16) | −0.0017 (14) |
C18 | 0.043 (2) | 0.0220 (18) | 0.047 (2) | 0.0039 (16) | 0.0012 (19) | −0.0002 (16) |
C19 | 0.030 (2) | 0.030 (2) | 0.038 (2) | 0.0000 (15) | −0.0069 (16) | −0.0002 (16) |
C20 | 0.0326 (19) | 0.0226 (17) | 0.0241 (17) | −0.0065 (14) | 0.0013 (15) | −0.0010 (13) |
C21 | 0.0265 (18) | 0.0251 (18) | 0.0253 (17) | −0.0017 (14) | 0.0038 (15) | −0.0057 (14) |
O7 | 0.0325 (15) | 0.0290 (14) | 0.0265 (13) | 0.0058 (11) | 0.0053 (11) | 0.0007 (11) |
Ho—O3 | 2.337 (2) | C3—C4 | 1.388 (4) |
Ho—O4i | 2.364 (2) | C4—C5 | 1.382 (5) |
Ho—O1 | 2.371 (2) | C4—H4 | 0.9300 |
Ho—O2ii | 2.379 (2) | C5—C6 | 1.403 (4) |
Ho—O6 | 2.478 (2) | C5—H5 | 0.9300 |
Ho—O5 | 2.482 (2) | C6—C7 | 1.487 (4) |
Ho—O7 | 2.546 (2) | C8—C9 | 1.380 (5) |
Ho—N1iii | 2.691 (3) | C8—C13 | 1.391 (5) |
O1—C7 | 1.257 (4) | C8—H8 | 0.9300 |
O2—C7 | 1.270 (4) | C9—C10 | 1.382 (5) |
O2—Hoii | 2.379 (2) | C9—H9 | 0.9300 |
O3—C14 | 1.254 (4) | C10—C11 | 1.390 (5) |
O4—C14 | 1.263 (4) | C11—C12 | 1.364 (5) |
O4—Hoi | 2.364 (2) | C11—H11 | 0.9300 |
O5—C21 | 1.262 (4) | C12—C13 | 1.393 (4) |
O6—C21 | 1.270 (4) | C12—H12 | 0.9300 |
N1—C3 | 1.417 (4) | C13—C14 | 1.482 (4) |
N1—Hoiii | 2.691 (3) | C15—C16 | 1.379 (4) |
N1—H1A | 0.861 (10) | C15—C20 | 1.390 (5) |
N1—H1B | 0.850 (10) | C15—H15 | 0.9300 |
N2—C10 | 1.389 (5) | C16—C17 | 1.392 (5) |
N2—H2A | 0.849 (10) | C16—H16 | 0.9300 |
N2—H2B | 0.851 (10) | C17—C18 | 1.384 (5) |
N3—C17 | 1.405 (4) | C18—C19 | 1.382 (5) |
N3—H3A | 0.858 (10) | C18—H18 | 0.9300 |
N3—H3B | 0.856 (10) | C19—C20 | 1.383 (5) |
C1—C2 | 1.371 (4) | C19—H19 | 0.9300 |
C1—C6 | 1.383 (4) | C20—C21 | 1.488 (4) |
C1—H1 | 0.9300 | O7—H7A | 0.817 (10) |
C2—C3 | 1.395 (4) | O7—H7B | 0.816 (10) |
C2—H2 | 0.9300 | ||
O3—Ho—O4i | 105.32 (8) | C2—C3—N1 | 120.5 (3) |
O3—Ho—O1 | 93.52 (8) | C5—C4—C3 | 120.5 (3) |
O4i—Ho—O1 | 142.40 (8) | C5—C4—H4 | 119.8 |
O3—Ho—O2ii | 147.74 (8) | C3—C4—H4 | 119.8 |
O4i—Ho—O2ii | 88.18 (8) | C4—C5—C6 | 120.2 (3) |
O1—Ho—O2ii | 92.87 (8) | C4—C5—H5 | 119.9 |
O3—Ho—O6 | 77.16 (8) | C6—C5—H5 | 119.9 |
O4i—Ho—O6 | 89.61 (8) | C1—C6—C5 | 118.7 (3) |
O1—Ho—O6 | 126.70 (7) | C1—C6—C7 | 121.3 (3) |
O2ii—Ho—O6 | 73.72 (7) | C5—C6—C7 | 120.0 (3) |
O3—Ho—O5 | 79.32 (8) | O1—C7—O2 | 122.4 (3) |
O4i—Ho—O5 | 140.61 (8) | O1—C7—C6 | 118.7 (3) |
O1—Ho—O5 | 74.09 (7) | O2—C7—C6 | 118.9 (3) |
O2ii—Ho—O5 | 72.15 (8) | C9—C8—C13 | 121.0 (3) |
O6—Ho—O5 | 52.62 (7) | C9—C8—H8 | 119.5 |
O3—Ho—O7 | 138.60 (8) | C13—C8—H8 | 119.5 |
O4i—Ho—O7 | 69.67 (8) | C8—C9—C10 | 120.8 (3) |
O1—Ho—O7 | 74.66 (8) | C8—C9—H9 | 119.6 |
O2ii—Ho—O7 | 73.43 (8) | C10—C9—H9 | 119.6 |
O6—Ho—O7 | 141.40 (8) | C9—C10—N2 | 121.0 (4) |
O5—Ho—O7 | 131.53 (7) | C9—C10—C11 | 118.2 (3) |
O3—Ho—N1iii | 69.98 (8) | N2—C10—C11 | 120.8 (4) |
O4i—Ho—N1iii | 75.45 (9) | C12—C11—C10 | 121.1 (3) |
O1—Ho—N1iii | 81.16 (8) | C12—C11—H11 | 119.4 |
O2ii—Ho—N1iii | 142.27 (8) | C10—C11—H11 | 119.4 |
O6—Ho—N1iii | 138.27 (8) | C11—C12—C13 | 121.2 (3) |
O5—Ho—N1iii | 138.98 (8) | C11—C12—H12 | 119.4 |
O7—Ho—N1iii | 69.05 (8) | C13—C12—H12 | 119.4 |
O3—Ho—C21 | 75.52 (9) | C8—C13—C12 | 117.6 (3) |
O4i—Ho—C21 | 115.69 (9) | C8—C13—C14 | 121.5 (3) |
O1—Ho—C21 | 100.27 (9) | C12—C13—C14 | 120.8 (3) |
O2ii—Ho—C21 | 72.24 (8) | O3—C14—O4 | 121.7 (3) |
O6—Ho—C21 | 26.44 (8) | O3—C14—C13 | 119.6 (3) |
O5—Ho—C21 | 26.24 (8) | O4—C14—C13 | 118.7 (3) |
O7—Ho—C21 | 144.97 (9) | C16—C15—C20 | 120.6 (3) |
N1iii—Ho—C21 | 145.48 (9) | C16—C15—H15 | 119.7 |
C7—O1—Ho | 137.4 (2) | C20—C15—H15 | 119.7 |
C7—O2—Hoii | 145.5 (2) | C15—C16—C17 | 120.7 (3) |
C14—O3—Ho | 150.8 (2) | C15—C16—H16 | 119.6 |
C14—O4—Hoi | 122.2 (2) | C17—C16—H16 | 119.6 |
C21—O5—Ho | 93.32 (19) | C18—C17—C16 | 118.7 (3) |
C21—O6—Ho | 93.30 (18) | C18—C17—N3 | 120.9 (3) |
C3—N1—Hoiii | 118.1 (2) | C16—C17—N3 | 120.4 (3) |
C3—N1—H1A | 111 (2) | C19—C18—C17 | 120.4 (3) |
Hoiii—N1—H1A | 105 (2) | C19—C18—H18 | 119.8 |
C3—N1—H1B | 111 (2) | C17—C18—H18 | 119.8 |
Hoiii—N1—H1B | 103 (2) | C18—C19—C20 | 121.2 (3) |
H1A—N1—H1B | 109 (3) | C18—C19—H19 | 119.4 |
C10—N2—H2A | 113 (3) | C20—C19—H19 | 119.4 |
C10—N2—H2B | 117 (4) | C19—C20—C15 | 118.5 (3) |
H2A—N2—H2B | 111.4 (18) | C19—C20—C21 | 120.4 (3) |
C17—N3—H3A | 112 (2) | C15—C20—C21 | 121.1 (3) |
C17—N3—H3B | 112 (3) | O5—C21—O6 | 120.5 (3) |
H3A—N3—H3B | 108.6 (16) | O5—C21—C20 | 119.9 (3) |
C2—C1—C6 | 121.2 (3) | O6—C21—C20 | 119.6 (3) |
C2—C1—H1 | 119.4 | O5—C21—Ho | 60.44 (16) |
C6—C1—H1 | 119.4 | O6—C21—Ho | 60.26 (16) |
C1—C2—C3 | 120.4 (3) | C20—C21—Ho | 174.2 (2) |
C1—C2—H2 | 119.8 | Ho—O7—H7A | 120 (3) |
C3—C2—H2 | 119.8 | Ho—O7—H7B | 104 (3) |
C4—C3—C2 | 119.0 (3) | H7A—O7—H7B | 110 (4) |
C4—C3—N1 | 120.4 (3) | ||
O3—Ho—O1—C7 | −167.7 (3) | C13—C8—C9—C10 | 0.5 (6) |
O4i—Ho—O1—C7 | −46.8 (4) | C8—C9—C10—N2 | −177.6 (4) |
O2ii—Ho—O1—C7 | 44.0 (3) | C8—C9—C10—C11 | 2.3 (6) |
O6—Ho—O1—C7 | 115.8 (3) | C9—C10—C11—C12 | −3.5 (6) |
O5—Ho—O1—C7 | 114.5 (3) | N2—C10—C11—C12 | 176.4 (4) |
O7—Ho—O1—C7 | −28.0 (3) | C10—C11—C12—C13 | 1.9 (6) |
N1iii—Ho—O1—C7 | −98.6 (3) | C9—C8—C13—C12 | −2.2 (6) |
C21—Ho—O1—C7 | 116.4 (3) | C9—C8—C13—C14 | 175.2 (3) |
O4i—Ho—O3—C14 | 116.5 (5) | C11—C12—C13—C8 | 1.0 (6) |
O1—Ho—O3—C14 | −96.4 (5) | C11—C12—C13—C14 | −176.4 (3) |
O2ii—Ho—O3—C14 | 4.7 (5) | Ho—O3—C14—O4 | −107.2 (5) |
O6—Ho—O3—C14 | 30.5 (5) | Ho—O3—C14—C13 | 71.2 (6) |
O5—Ho—O3—C14 | −23.3 (4) | Hoi—O4—C14—O3 | 1.3 (4) |
O7—Ho—O3—C14 | −167.0 (4) | Hoi—O4—C14—C13 | −177.1 (2) |
N1iii—Ho—O3—C14 | −175.6 (5) | C8—C13—C14—O3 | −169.8 (3) |
C21—Ho—O3—C14 | 3.3 (4) | C12—C13—C14—O3 | 7.5 (5) |
O3—Ho—O5—C21 | 78.9 (2) | C8—C13—C14—O4 | 8.7 (5) |
O4i—Ho—O5—C21 | −22.3 (2) | C12—C13—C14—O4 | −174.1 (3) |
O1—Ho—O5—C21 | 175.7 (2) | C20—C15—C16—C17 | 0.4 (5) |
O2ii—Ho—O5—C21 | −85.9 (2) | C15—C16—C17—C18 | −0.3 (5) |
O6—Ho—O5—C21 | −3.06 (18) | C15—C16—C17—N3 | −179.3 (3) |
O7—Ho—O5—C21 | −132.63 (19) | C16—C17—C18—C19 | −0.1 (5) |
N1iii—Ho—O5—C21 | 120.5 (2) | N3—C17—C18—C19 | 178.9 (3) |
O3—Ho—O6—C21 | −83.24 (19) | C17—C18—C19—C20 | 0.4 (6) |
O4i—Ho—O6—C21 | 170.95 (19) | C18—C19—C20—C15 | −0.3 (5) |
O1—Ho—O6—C21 | 1.5 (2) | C18—C19—C20—C21 | 179.4 (3) |
O2ii—Ho—O6—C21 | 82.74 (19) | C16—C15—C20—C19 | −0.1 (5) |
O5—Ho—O6—C21 | 3.04 (18) | C16—C15—C20—C21 | −179.8 (3) |
O7—Ho—O6—C21 | 115.4 (2) | Ho—O5—C21—O6 | 5.5 (3) |
N1iii—Ho—O6—C21 | −121.70 (19) | Ho—O5—C21—C20 | −173.3 (3) |
C6—C1—C2—C3 | 2.2 (5) | Ho—O6—C21—O5 | −5.5 (3) |
C1—C2—C3—C4 | −1.8 (5) | Ho—O6—C21—C20 | 173.3 (3) |
C1—C2—C3—N1 | 174.7 (3) | C19—C20—C21—O5 | 20.0 (5) |
Hoiii—N1—C3—C4 | 92.5 (3) | C15—C20—C21—O5 | −160.3 (3) |
Hoiii—N1—C3—C2 | −83.9 (3) | C19—C20—C21—O6 | −158.8 (3) |
C2—C3—C4—C5 | 0.4 (5) | C15—C20—C21—O6 | 20.8 (5) |
N1—C3—C4—C5 | −176.1 (3) | O3—Ho—C21—O5 | −95.2 (2) |
C3—C4—C5—C6 | 0.6 (5) | O4i—Ho—C21—O5 | 164.48 (17) |
C2—C1—C6—C5 | −1.2 (5) | O1—Ho—C21—O5 | −4.2 (2) |
C2—C1—C6—C7 | −178.1 (3) | O2ii—Ho—C21—O5 | 85.51 (19) |
C4—C5—C6—C1 | −0.2 (5) | O6—Ho—C21—O5 | 174.5 (3) |
C4—C5—C6—C7 | 176.7 (3) | O7—Ho—C21—O5 | 73.7 (2) |
Ho—O1—C7—O2 | −11.6 (5) | N1iii—Ho—C21—O5 | −93.5 (2) |
Ho—O1—C7—C6 | 167.5 (2) | O3—Ho—C21—O6 | 90.23 (19) |
Hoii—O2—C7—O1 | −91.0 (4) | O4i—Ho—C21—O6 | −10.1 (2) |
Hoii—O2—C7—C6 | 89.9 (4) | O1—Ho—C21—O6 | −178.77 (18) |
C1—C6—C7—O1 | 5.5 (4) | O2ii—Ho—C21—O6 | −89.03 (19) |
C5—C6—C7—O1 | −171.3 (3) | O5—Ho—C21—O6 | −174.5 (3) |
C1—C6—C7—O2 | −175.3 (3) | O7—Ho—C21—O6 | −100.9 (2) |
C5—C6—C7—O2 | 7.8 (4) | N1iii—Ho—C21—O6 | 91.9 (2) |
Symmetry codes: (i) −x+1, −y+1, −z+2; (ii) −x+1, −y+1, −z+1; (iii) −x, −y+1, −z+1. |
D—H···A | D—H | H···A | D···A | D—H···A |
N1—H1A···O6iv | 0.86 (1) | 2.05 (1) | 2.902 (3) | 172 (3) |
N1—H1B···N2v | 0.85 (1) | 2.51 (1) | 3.360 (5) | 177 (3) |
N2—H2A···O7vi | 0.85 (1) | 2.43 (3) | 3.139 (5) | 142 (3) |
N3—H3A···O5vii | 0.86 (1) | 2.23 (2) | 2.974 (4) | 145 (3) |
O7—H7B···O2 | 0.82 (1) | 2.00 (2) | 2.773 (3) | 158 (4) |
O7—H7A···N3viii | 0.82 (1) | 2.08 (2) | 2.875 (4) | 165 (5) |
Symmetry codes: (iv) x−1, y, z−1; (v) x−1/2, −y+3/2, z−1/2; (vi) −x+1/2, y+1/2, −z+3/2; (vii) x+1/2, −y+3/2, z+1/2; (viii) −x+3/2, y−1/2, −z+3/2. |
Experimental details
Crystal data | |
Chemical formula | [Ho(C7H6NO2)3(H2O)] |
Mr | 591.33 |
Crystal system, space group | Monoclinic, P21/n |
Temperature (K) | 294 |
a, b, c (Å) | 9.772 (1), 22.761 (3), 9.832 (1) |
β (°) | 100.02 (1) |
V (Å3) | 2153.5 (4) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 3.72 |
Crystal size (mm) | 0.24 × 0.20 × 0.18 |
Data collection | |
Diffractometer | Bruker SMART CCD area-detector |
Absorption correction | Multi-scan (SADABS; Sheldrick, 2003) |
Tmin, Tmax | 0.413, 0.512 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 4521, 4001, 2954 |
Rint | 0.014 |
(sin θ/λ)max (Å−1) | 0.606 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.021, 0.052, 1.03 |
No. of reflections | 4005 |
No. of parameters | 322 |
No. of restraints | 10 |
H-atom treatment | H atoms treated by a mixture of independent and constrained refinement |
Δρmax, Δρmin (e Å−3) | 0.44, −0.53 |
Computer programs: SMART (Bruker, 2001), SMART, SAINT (Bruker, 2003), SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), SHELXTL (Sheldrick, 2003), SHELXTL.
D—H···A | D—H | H···A | D···A | D—H···A |
N1—H1A···O6i | 0.861 (10) | 2.046 (12) | 2.902 (3) | 172 (3) |
N1—H1B···N2ii | 0.850 (10) | 2.510 (11) | 3.360 (5) | 177 (3) |
N2—H2A···O7iii | 0.849 (10) | 2.43 (3) | 3.139 (5) | 142 (3) |
N3—H3A···O5iv | 0.858 (10) | 2.23 (2) | 2.974 (4) | 145 (3) |
O7—H7B···O2 | 0.816 (10) | 2.000 (18) | 2.773 (3) | 158 (4) |
O7—H7A···N3v | 0.817 (10) | 2.079 (16) | 2.875 (4) | 165 (5) |
Symmetry codes: (i) x−1, y, z−1; (ii) x−1/2, −y+3/2, z−1/2; (iii) −x+1/2, y+1/2, −z+3/2; (iv) x+1/2, −y+3/2, z+1/2; (v) −x+3/2, y−1/2, −z+3/2. |
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During the last two decades, lanthanide complexes have received much attention because of their interesting photophysical properties which have potential applications in the luminescent probes for chemical or biological macromolecules and the active center for luminescent materials(Chu et al., 2001; Kepert & Rosseinsky, 1998; Reineke et al., 1999; Chen et al., 2006;). We have chosen 4-aminobenzonitrile as ligand and investigated its reaction with Ho2O3 under hydrothermal synthesis, and report herein the X-ray crystal structure of the novel terbium coordination polymer, [Ho(4-aminobenzoate)3(H2O)]n, (I).
In (I) (Fig. 1), the HoIII center is eight-coordinated by six O atoms from five different 4-aminobenzoate ligands, one N atoms from a 4-aminobenzoate ligand and one O atoms from a coordinated water molecule, thus the HoIII ion has a distorted bicapped trigonal prism. In the coordination polyhedron of HoIII ion, the Ho—O distance of carboxyl is in the range 2.337 (2)–2.482 (2) Å, and the mean Ho—O bond length is 2.428 (2) Å. The Ho—O bond length involving the coordination water is 2.546 (2) Å, and the Ho—N distance is 2.691 (3) Å. In (I), each 4-aminobenzoate ligand adopts an O,O-bidentate bridging mode using a carboxylate group. Adjacent HoIII centers are doubly bridged by the ligands, forming a big eight-membered ring, while the other two Ho atoms has a 16-membered ring bridged by the carboxylate groups and amino groups (Fig. 2).