The asymmetric unit of the title compound, [Er(C6H3ClNO2)3(H2O)2]n, has two independent disordered 2-chloronicotinate groups, one of which lies on a twofold rotation axis. The group lying on this symmetry element chelates to the water-coordinated Er atom, which also lies on the rotation axis. Two more 2-chloronicotinate groups bridge two diaqua(2-chloronicotinato)erbium species into a linear chain. The Er atom exists in a square-antiprismatic environment made up of O atoms.
Supporting information
CCDC reference: 289945
Key indicators
- Single-crystal X-ray study
- T = 295 K
- Mean (O-C) = 0.006 Å
- Disorder in main residue
- R factor = 0.039
- wR factor = 0.089
- Data-to-parameter ratio = 12.0
checkCIF/PLATON results
No syntax errors found
Alert level A
ABSTM02_ALERT_3_A The ratio of expected to reported Tmax/Tmin(RR') is < 0.50
Tmin and Tmax reported: 0.170 0.672
Tmin(prime) and Tmax expected: 0.640 0.649
RR(prime) = 0.256
Please check that your absorption correction is appropriate.
PLAT061_ALERT_3_A Tmax/Tmin Range Test RR' too Large ............. 0.25
Alert level B
PLAT301_ALERT_3_B Main Residue Disorder ......................... 39.00 Perc.
Alert level C
PLAT062_ALERT_4_C Rescale T(min) & T(max) by ..................... 0.96
PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for Er1
PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 2
2 ALERT level A = In general: serious problem
1 ALERT level B = Potentially serious problem
3 ALERT level C = Check and explain
0 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
3 ALERT type 3 Indicator that the structure quality may be low
2 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: RAPID AUTO (Rigaku, 1998); cell refinement: RAPID AUTO; data reduction: CrystalStructure (Rigaku/MSC, 2002); 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.
catena-Poly[[diaqua(2-chloronicotinato-
κ2O,
O')erbium(III)]-di-µ-2- chloronicotinato-
κ4O:
O']
top
Crystal data top
[Er(C6H3ClNO2)3(H2O)2] | F(000) = 1300 |
Mr = 672.92 | Dx = 2.078 Mg m−3 |
Monoclinic, C2/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -C 2yc | Cell parameters from 9329 reflections |
a = 16.324 (3) Å | θ = 3.1–27.5° |
b = 14.130 (3) Å | µ = 4.33 mm−1 |
c = 9.614 (2) Å | T = 295 K |
β = 104.05 (3)° | Prism, pink |
V = 2151.2 (8) Å3 | 0.10 × 0.10 × 0.10 mm |
Z = 4 | |
Data collection top
Rigaku R-AXIS RAPID IP diffractometer | 2464 independent reflections |
Radiation source: fine-focus sealed tube | 2317 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.066 |
ω scans | θmax = 27.5°, θmin = 3.1° |
Absorption correction: multi-scan (ABSCOR; Higashi, 1995) | h = −21→21 |
Tmin = 0.170, Tmax = 0.672 | k = −18→18 |
10139 measured reflections | l = −11→12 |
Refinement top
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)] = 0.039 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.089 | H-atom parameters constrained |
S = 1.14 | w = 1/[σ2(Fo2) + (0.035P)2 + 5.2256P] where P = (Fo2 + 2Fc2)/3 |
2464 reflections | (Δ/σ)max = 0.001 |
205 parameters | Δρmax = 1.60 e Å−3 |
62 restraints | Δρmin = −1.81 e Å−3 |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | Occ. (<1) |
Er1 | 0.5000 | 0.51055 (2) | 0.7500 | 0.02379 (12) | |
Cl1 | 0.2820 (2) | 0.7259 (3) | 0.2022 (4) | 0.0482 (9) | 0.53 (1) |
N1 | 0.1607 (14) | 0.710 (2) | 0.331 (3) | 0.042 (2) | 0.53 (1) |
C1 | 0.2353 (14) | 0.6741 (19) | 0.328 (2) | 0.032 (3) | 0.53 (1) |
C2 | 0.2762 (8) | 0.6034 (14) | 0.418 (2) | 0.0269 (14) | 0.53 (1) |
C3 | 0.2378 (8) | 0.5667 (9) | 0.5197 (16) | 0.035 (3) | 0.53 (1) |
H3 | 0.2639 | 0.5193 | 0.5820 | 0.041* | 0.53 (1) |
C4 | 0.1600 (8) | 0.6019 (8) | 0.5271 (14) | 0.042 (2) | 0.53 (1) |
H4 | 0.1318 | 0.5793 | 0.5935 | 0.051* | 0.53 (1) |
C5 | 0.1268 (19) | 0.6719 (12) | 0.431 (2) | 0.048 (3) | 0.53 (1) |
H5 | 0.0745 | 0.6955 | 0.4368 | 0.057* | 0.53 (1) |
Cl1' | 0.2605 (3) | 0.6826 (3) | 0.1677 (4) | 0.0482 (9) | 0.47 |
N1' | 0.1586 (16) | 0.701 (2) | 0.331 (4) | 0.042 (2) | 0.47 |
C1' | 0.2296 (16) | 0.657 (2) | 0.324 (2) | 0.032 (3) | 0.47 |
C2' | 0.2777 (9) | 0.6016 (16) | 0.432 (2) | 0.0269 (14) | 0.47 |
C3' | 0.2440 (9) | 0.5959 (10) | 0.5508 (19) | 0.035 (3) | 0.47 |
H3' | 0.2727 | 0.5601 | 0.6287 | 0.041* | 0.47 (1) |
C4' | 0.1700 (9) | 0.6405 (9) | 0.5603 (16) | 0.042 (2) | 0.47 |
H4' | 0.1495 | 0.6341 | 0.6420 | 0.051* | 0.47 (1) |
C5' | 0.127 (2) | 0.6942 (14) | 0.447 (3) | 0.048 (3) | 0.47 |
H5' | 0.0778 | 0.7253 | 0.4510 | 0.057* | 0.47 (1) |
O1W | 0.4422 (2) | 0.6464 (3) | 0.8376 (4) | 0.0444 (10) | |
H1W1 | 0.3962 | 0.6589 | 0.7841 | 0.053* | |
H1W2 | 0.4363 | 0.6356 | 0.9184 | 0.053* | |
O1 | 0.4106 (2) | 0.5458 (3) | 0.5405 (4) | 0.0402 (9) | |
O2 | 0.3754 (2) | 0.5407 (3) | 0.3032 (4) | 0.0424 (9) | |
C6 | 0.3607 (3) | 0.5596 (3) | 0.4203 (5) | 0.0290 (10) | |
Cl2 | 0.4057 (2) | 0.1676 (2) | 0.5077 (3) | 0.0494 (7) | 0.50 |
O3 | 0.4722 (2) | 0.3554 (3) | 0.6345 (3) | 0.0390 (9) | |
C7 | 0.5000 | 0.3113 (5) | 0.7500 | 0.0321 (15) | |
C8 | 0.5133 (6) | 0.2055 (6) | 0.7689 (12) | 0.026 (3) | 0.50 |
C9 | 0.4703 (5) | 0.1401 (6) | 0.6687 (9) | 0.032 (2) | 0.50 |
N2 | 0.4764 (9) | 0.0445 (6) | 0.6927 (13) | 0.045 (3) | 0.50 |
C10 | 0.5268 (11) | 0.0122 (7) | 0.8204 (16) | 0.054 (5) | 0.50 |
H10 | 0.5313 | −0.0526 | 0.8376 | 0.065* | 0.50 |
C11 | 0.5710 (7) | 0.0742 (7) | 0.9238 (11) | 0.055 (3) | 0.50 |
H11 | 0.6047 | 0.0515 | 1.0095 | 0.065* | 0.50 |
C12 | 0.5639 (6) | 0.1709 (7) | 0.8966 (11) | 0.037 (2) | 0.50 |
H12 | 0.5933 | 0.2130 | 0.9650 | 0.044* | 0.50 |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Er1 | 0.02104 (18) | 0.02505 (18) | 0.02415 (17) | 0.000 | 0.00326 (12) | 0.000 |
Cl1 | 0.0470 (18) | 0.060 (2) | 0.0394 (16) | 0.0135 (15) | 0.0145 (13) | 0.0224 (15) |
N1 | 0.038 (2) | 0.040 (5) | 0.047 (3) | 0.014 (3) | 0.012 (2) | 0.008 (3) |
C1 | 0.035 (3) | 0.032 (8) | 0.029 (3) | 0.005 (4) | 0.011 (2) | 0.003 (4) |
C2 | 0.027 (2) | 0.031 (3) | 0.021 (3) | −0.0004 (19) | 0.004 (2) | −0.001 (2) |
C3 | 0.032 (3) | 0.037 (7) | 0.035 (6) | −0.003 (4) | 0.009 (3) | 0.002 (5) |
C4 | 0.040 (4) | 0.045 (7) | 0.046 (5) | −0.007 (5) | 0.018 (4) | −0.002 (5) |
C5 | 0.034 (3) | 0.053 (8) | 0.060 (5) | 0.012 (6) | 0.018 (4) | −0.007 (6) |
Cl1' | 0.0470 (18) | 0.060 (2) | 0.0394 (16) | 0.0135 (15) | 0.0145 (13) | 0.0224 (15) |
N1' | 0.038 (2) | 0.040 (5) | 0.047 (3) | 0.014 (3) | 0.012 (2) | 0.008 (3) |
C1' | 0.035 (3) | 0.032 (8) | 0.029 (3) | 0.005 (4) | 0.011 (2) | 0.003 (4) |
C2' | 0.027 (2) | 0.031 (3) | 0.021 (3) | −0.0004 (19) | 0.004 (2) | −0.001 (2) |
C3' | 0.032 (3) | 0.037 (7) | 0.035 (6) | −0.003 (4) | 0.009 (3) | 0.002 (5) |
C4' | 0.040 (4) | 0.045 (7) | 0.046 (5) | −0.007 (5) | 0.018 (4) | −0.002 (5) |
C5' | 0.034 (3) | 0.053 (8) | 0.060 (5) | 0.012 (6) | 0.018 (4) | −0.007 (6) |
O1W | 0.058 (2) | 0.044 (2) | 0.0345 (19) | 0.0254 (19) | 0.0170 (17) | 0.0110 (17) |
O1 | 0.0257 (17) | 0.047 (2) | 0.041 (2) | −0.0010 (17) | −0.0055 (15) | 0.0183 (18) |
O2 | 0.0307 (19) | 0.052 (2) | 0.042 (2) | 0.0080 (18) | 0.0037 (15) | −0.0203 (19) |
C6 | 0.026 (2) | 0.022 (2) | 0.036 (2) | −0.0011 (18) | 0.0012 (19) | 0.0012 (19) |
Cl2 | 0.0655 (19) | 0.0333 (15) | 0.0399 (15) | −0.0071 (13) | −0.0057 (14) | −0.0044 (12) |
O3 | 0.057 (2) | 0.029 (2) | 0.0251 (17) | −0.0142 (17) | −0.0009 (15) | 0.0033 (14) |
C7 | 0.043 (4) | 0.029 (4) | 0.027 (3) | 0.000 | 0.013 (3) | 0.000 |
C8 | 0.018 (8) | 0.030 (4) | 0.029 (8) | 0.007 (4) | 0.008 (6) | 0.000 (5) |
C9 | 0.030 (6) | 0.026 (6) | 0.041 (6) | −0.004 (4) | 0.011 (5) | 0.000 (5) |
N2 | 0.061 (8) | 0.009 (6) | 0.062 (7) | −0.008 (6) | 0.008 (5) | −0.004 (5) |
C10 | 0.069 (11) | 0.014 (8) | 0.072 (10) | 0.007 (8) | 0.003 (8) | 0.014 (8) |
C11 | 0.065 (8) | 0.041 (7) | 0.055 (7) | 0.017 (6) | 0.009 (6) | 0.016 (6) |
C12 | 0.030 (6) | 0.032 (6) | 0.043 (7) | 0.002 (5) | 0.001 (5) | 0.000 (5) |
Geometric parameters (Å, º) top
Er1—O1 | 2.237 (3) | C2'—C6 | 1.507 (8) |
Er1—O1i | 2.237 (3) | C3'—C4' | 1.385 (10) |
Er1—O2ii | 2.330 (3) | C3'—H3' | 0.9300 |
Er1—O2iii | 2.330 (3) | C4'—C5' | 1.368 (12) |
Er1—O3 | 2.450 (4) | C4'—H4' | 0.9300 |
Er1—O3i | 2.450 (4) | C5'—H5' | 0.9300 |
Er1—O1W | 2.381 (4) | O1W—H1W1 | 0.8200 |
Er1—O1Wi | 2.381 (4) | O1W—H1W2 | 0.8200 |
Cl1—C1 | 1.737 (9) | O1—C6 | 1.257 (6) |
N1—C1 | 1.330 (8) | O2—C6 | 1.236 (6) |
N1—C5 | 1.337 (10) | Cl2—C9 | 1.693 (9) |
C1—C2 | 1.383 (8) | O3—C7 | 1.258 (5) |
C2—C3 | 1.386 (9) | C7—O3i | 1.258 (5) |
C2—C6 | 1.506 (8) | C7—C8 | 1.515 (11) |
C3—C4 | 1.382 (10) | C7—C8i | 1.515 (11) |
C3—H3 | 0.9300 | C8—C12 | 1.392 (8) |
C4—C5 | 1.369 (11) | C8—C9 | 1.396 (8) |
C4—H4 | 0.9300 | C9—N2 | 1.370 (8) |
C5—H5 | 0.9300 | N2—C10 | 1.379 (8) |
Cl1'—C1' | 1.737 (9) | C10—C11 | 1.389 (9) |
N1'—C1' | 1.330 (8) | C10—H10 | 0.9300 |
N1'—C5' | 1.336 (11) | C11—C12 | 1.390 (8) |
C1'—C2' | 1.383 (9) | C11—H11 | 0.9300 |
C2'—C3' | 1.387 (10) | C12—H12 | 0.9300 |
| | | |
O1—Er1—O1i | 154.3 (2) | C4'—C3'—H3' | 118.1 |
O1—Er1—O2ii | 106.5 (1) | C2'—C3'—H3' | 118.1 |
O1—Er1—O2iii | 81.6 (1) | C5'—C4'—C3' | 119 (2) |
O1—Er1—O3 | 77.5 (1) | C5'—C4'—H4' | 120.6 |
O1—Er1—O3i | 128.0 (1) | C3'—C4'—H4' | 120.6 |
O1—Er1—O1W | 84.9 (2) | N1'—C5'—C4' | 119 (3) |
O1—Er1—O1Wi | 74.3 (1) | N1'—C5'—H5' | 120.6 |
O2ii—Er1—O2iii | 143.8 (2) | C4'—C5'—H5' | 120.6 |
O2ii—Er1—O3 | 72.4 (1) | Er1—O1W—H1W1 | 109.5 |
O2ii—Er1—O3i | 75.3 (2) | Er1—O1W—H1W2 | 109.5 |
O2ii—Er1—O1W | 140.4 (2) | H1W1—O1W—H1W2 | 109.5 |
O2ii—Er1—O1Wi | 74.4 (2) | C6—O1—Er1 | 175.9 (4) |
O3—Er1—O3i | 53.0 (2) | C6—O2—Er1ii | 129.8 (3) |
O3—Er1—O1W | 146.8 (1) | O2—C6—O1 | 125.3 (4) |
O3—Er1—O1Wi | 127.3 (1) | O2—C6—C2 | 116.9 (8) |
O1W—Er1—O1Wi | 72.6 (2) | O1—C6—C2 | 117.8 (8) |
C1—N1—C5 | 114 (3) | O2—C6—C2' | 121.9 (9) |
N1—C1—C2 | 124.6 (17) | O1—C6—C2' | 112.8 (9) |
N1—C1—Cl1 | 114.5 (17) | C7—O3—Er1 | 93.2 (3) |
C2—C1—Cl1 | 120.8 (15) | O3i—C7—O3 | 120.7 (7) |
C1—C2—C3 | 118.7 (10) | O3i—C7—C8 | 111.9 (5) |
C1—C2—C6 | 127.5 (15) | O3—C7—C8 | 127.2 (5) |
C3—C2—C6 | 113.8 (11) | O3i—C7—C8i | 127.2 (5) |
C4—C3—C2 | 118.7 (12) | O3—C7—C8i | 111.9 (5) |
C4—C3—H3 | 120.6 | C12—C8—C9 | 117.8 (8) |
C2—C3—H3 | 120.6 | C12—C8—C7 | 119.3 (7) |
C5—C4—C3 | 116.4 (18) | C9—C8—C7 | 122.6 (7) |
C5—C4—H4 | 121.8 | N2—C9—C8 | 122.2 (9) |
C3—C4—H4 | 121.8 | N2—C9—Cl2 | 112.6 (7) |
N1—C5—C4 | 128 (3) | C8—C9—Cl2 | 125.2 (7) |
N1—C5—H5 | 116.1 | C9—N2—C10 | 118.7 (8) |
C4—C5—H5 | 116.1 | N2—C10—C11 | 121.5 (8) |
C1'—N1'—C5' | 121 (3) | N2—C10—H10 | 119.3 |
N1'—C1'—C2' | 124.8 (19) | C11—C10—H10 | 119.3 |
N1'—C1'—Cl1' | 112.8 (19) | C10—C11—C12 | 118.7 (9) |
C2'—C1'—Cl1' | 122.3 (16) | C10—C11—H11 | 120.6 |
C1'—C2'—C3' | 112.5 (11) | C12—C11—H11 | 120.6 |
C1'—C2'—C6 | 121.8 (17) | C11—C12—C8 | 121.1 (9) |
C3'—C2'—C6 | 125.6 (13) | C11—C12—H12 | 119.5 |
C4'—C3'—C2' | 123.7 (14) | C8—C12—H12 | 119.5 |
| | | |
C5—N1—C1—C2 | −0.1 (3) | C3'—C2'—C6—O1 | −22 (2) |
C5—N1—C1—Cl1 | −178 (2) | O1i—Er1—O3—C7 | 20.9 (3) |
N1—C1—C2—C3 | −0.1 (3) | O1—Er1—O3—C7 | −163.3 (2) |
Cl1—C1—C2—C3 | 178 (2) | O2iii—Er1—O3—C7 | −78.8 (2) |
N1—C1—C2—C6 | −179.6 (16) | O2ii—Er1—O3—C7 | 84.6 (2) |
Cl1—C1—C2—C6 | −1.9 (16) | O1Wi—Er1—O3—C7 | 137.91 (19) |
C1—C2—C3—C4 | 0.3 (7) | O1W—Er1—O3—C7 | −103.6 (2) |
C6—C2—C3—C4 | 179.9 (13) | O3i—Er1—O3—C7 | 0.000 (1) |
C2—C3—C4—C5 | −0.3 (9) | Er1—O3—C7—O3i | 0.0 |
C1—N1—C5—C4 | 0.1 (8) | Er1—O3—C7—C8 | −173.3 (6) |
C3—C4—C5—N1 | 0.1 (10) | Er1—O3—C7—C8i | 174.2 (5) |
C5'—N1'—C1'—C2' | 0.0 (3) | O3i—C7—C8—C12 | −10.1 (9) |
C5'—N1'—C1'—Cl1' | −176 (2) | O3—C7—C8—C12 | 163.7 (5) |
N1'—C1'—C2'—C3' | −0.2 (3) | C8i—C7—C8—C12 | −158 (4) |
Cl1'—C1'—C2'—C3' | 176 (2) | O3i—C7—C8—C9 | 163.5 (7) |
N1'—C1'—C2'—C6 | −175.7 (17) | O3—C7—C8—C9 | −22.7 (12) |
Cl1'—C1'—C2'—C6 | 0.4 (18) | C8i—C7—C8—C9 | 16 (2) |
C1'—C2'—C3'—C4' | 0.5 (7) | C12—C8—C9—N2 | 0.1 (3) |
C6—C2'—C3'—C4' | 175.8 (18) | C7—C8—C9—N2 | −173.6 (13) |
C2'—C3'—C4'—C5' | −0.7 (10) | C12—C8—C9—Cl2 | 179.8 (7) |
C1'—N1'—C5'—C4' | −0.1 (7) | C7—C8—C9—Cl2 | 6.1 (12) |
C3'—C4'—C5'—N1' | 0.5 (9) | C12i—Cl2—C9—N2 | 153 (3) |
Er1ii—O2—C6—O1 | −7.3 (8) | C11i—Cl2—C9—N2 | 0.8 (11) |
Er1ii—O2—C6—C2 | 172.2 (10) | C12i—Cl2—C9—C8 | −27 (3) |
Er1ii—O2—C6—C2' | 173.6 (11) | C11i—Cl2—C9—C8 | −178.9 (11) |
C1—C2—C6—O2 | −43.0 (12) | C8—C9—N2—C10 | 0.1 (3) |
C3—C2—C6—O2 | 137.5 (10) | Cl2—C9—N2—C10 | −179.7 (6) |
C1—C2—C6—O1 | 136.6 (9) | C9—N2—C10—C11 | −0.1 (7) |
C3—C2—C6—O1 | −42.9 (16) | N2—C10—C11—C12 | −0.1 (9) |
C1'—C2'—C6—O2 | −28.2 (14) | C10—C11—C12—C8 | 0.2 (9) |
C3'—C2'—C6—O2 | 156.8 (13) | C9—C8—C12—C11 | −0.3 (6) |
C1'—C2'—C6—O1 | 152.5 (10) | C7—C8—C12—C11 | 173.6 (11) |
Symmetry codes: (i) −x+1, y, −z+3/2; (ii) −x+1, −y+1, −z+1; (iii) x, −y+1, z+1/2. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O1W—H1W1···N1iv | 0.82 | 2.24 | 2.87 (3) | 134 |
O1W—H1W1···N1′iv | 0.82 | 2.34 | 2.95 (3) | 132 |
O1W—H1W2···O3iii | 0.82 | 2.02 | 2.776 (5) | 153 |
Symmetry codes: (iii) x, −y+1, z+1/2; (iv) −x+1/2, −y+3/2, −z+1. |