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The title compound, {K[Nd(C2O4)2(H2O)]·2H2O}n, has been prepared hydrothermally. Every NdIII atom is linked to four others through oxalate anions lying on centres of inversion, generating a three-dimensional anionic network with channels that contain K+ cations and water molecules.
Supporting information
CCDC reference: 636136
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (C-C) = 0.016 Å
- R factor = 0.054
- wR factor = 0.120
- Data-to-parameter ratio = 12.9
checkCIF/PLATON results
No syntax errors found
Alert level A
DIFF020_ALERT_1_A _diffrn_standards_interval_count and
_diffrn_standards_interval_time are missing. Number of measurements
between standards or time (min) between standards.
| Author Response: this is an image plate system
|
DIFF022_ALERT_1_A _diffrn_standards_decay_% is missing
Percentage decrease in standards intensity.
| Author Response: this is an image plate system
|
Alert level B
PLAT369_ALERT_2_B Long C(sp2)-C(sp2) Bond C3 - C3_b ... 1.59 Ang.
Alert level C
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ?
PLAT213_ALERT_2_C Atom O2 has ADP max/min Ratio ............. 3.10 prola
PLAT220_ALERT_2_C Large Non-Solvent O Ueq(max)/Ueq(min) ... 3.06 Ratio
PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for O2
PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for O7
PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for Nd1
PLAT342_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 16
PLAT369_ALERT_2_C Long C(sp2)-C(sp2) Bond C1 - C2 ... 1.54 Ang.
PLAT369_ALERT_2_C Long C(sp2)-C(sp2) Bond C4 - C4_j ... 1.53 Ang.
PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 6
PLAT764_ALERT_4_C Overcomplete CIF Bond List Detected (Rep/Expd) . 1.16 Ratio
Alert level G
FORMU01_ALERT_1_G There is a discrepancy between the atom counts in the
_chemical_formula_sum and _chemical_formula_moiety. This is
usually due to the moiety formula being in the wrong format.
Atom count from _chemical_formula_sum: C4 H6 K1 Nd1 O11
Atom count from _chemical_formula_moiety:C4 H8 K1 Nd1 O12
PLAT199_ALERT_1_G Check the Reported _cell_measurement_temperature 293 K
PLAT200_ALERT_1_G Check the Reported _diffrn_ambient_temperature . 293 K
2 ALERT level A = In general: serious problem
1 ALERT level B = Potentially serious problem
11 ALERT level C = Check and explain
3 ALERT level G = General alerts; check
6 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
8 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
2 ALERT type 4 Improvement, methodology, query or suggestion
0 ALERT type 5 Informative message, check
Data collection: PROCESS-AUTO (Rigaku, 1998); cell refinement: PROCESS-AUTO; data reduction: CrystalStructure (Rigaku/MSC, 2004); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: WinGX (Farrugia, 1999); software used to prepare material for publication: SHELXL97.
Poly[potassium aquadi-µ-oxalato-neodymium(III) dihydrate]
top
Crystal data top
K[Nd(C2O4)2(H2O)]·2H2O | F(000) = 1576 |
Mr = 413.43 | Dx = 2.487 Mg m−3 |
Monoclinic, C2/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -C 2yc | Cell parameters from 250 reflections |
a = 23.085 (5) Å | θ = 2.5–25° |
b = 7.4913 (15) Å | µ = 5.13 mm−1 |
c = 12.941 (3) Å | T = 293 K |
β = 99.286 (3)° | Block, pink |
V = 2208.6 (8) Å3 | 0.26 × 0.13 × 0.11 mm |
Z = 8 | |
Data collection top
Rigaku R-AXIS-IV diffractometer | 1985 independent reflections |
Radiation source: fine-focus sealed tube | 1531 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.041 |
ω scans | θmax = 25.3°, θmin = 3.2° |
Absorption correction: multi-scan (ABSCOR; Higashi, 1995) | h = −27→19 |
Tmin = 0.330, Tmax = 0.569 | k = −8→8 |
5056 measured reflections | l = −15→15 |
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)] = 0.054 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.120 | H-atom parameters constrained |
S = 1.28 | w = 1/[σ2(Fo2) + 55.1422P] where P = (Fo2 + 2Fc2)/3 |
1985 reflections | (Δ/σ)max < 0.001 |
154 parameters | Δρmax = 0.87 e Å−3 |
66 restraints | Δρmin = −2.08 e Å−3 |
Special details top
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. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
K1 | 0.58112 (15) | 0.0002 (5) | 0.8731 (3) | 0.0514 (8) | |
Nd1 | 0.63733 (2) | 0.50022 (9) | 0.51386 (4) | 0.0146 (2) | |
O1 | 0.6605 (4) | 0.6607 (13) | 0.8570 (6) | 0.041 (2) | |
O2 | 0.6703 (4) | 0.6413 (14) | 0.6886 (6) | 0.043 (2) | |
O3 | 0.5968 (4) | 0.3623 (11) | 0.8388 (6) | 0.0281 (19) | |
O4 | 0.5991 (3) | 0.3587 (10) | 0.6656 (6) | 0.0237 (18) | |
O5 | 0.5450 (3) | 0.3412 (10) | 0.4542 (5) | 0.0166 (16) | |
O6 | 0.4498 (3) | 0.3272 (10) | 0.4646 (6) | 0.0197 (17) | |
O7 | 0.7464 (4) | 0.5266 (11) | 0.5259 (8) | 0.039 (2) | |
O8 | 0.8239 (3) | 0.6983 (10) | 0.5122 (6) | 0.0228 (18) | |
C1 | 0.6510 (5) | 0.5883 (18) | 0.7694 (8) | 0.028 (3) | |
C2 | 0.6122 (5) | 0.4200 (14) | 0.7579 (8) | 0.013 (2) | |
C3 | 0.4985 (5) | 0.4023 (14) | 0.4762 (7) | 0.016 (2) | |
C4 | 0.7703 (4) | 0.6689 (15) | 0.5105 (8) | 0.019 (2) | |
O1W | 0.6766 (4) | 0.2032 (11) | 0.5566 (7) | 0.032 (2) | |
H1WA | 0.6814 | 0.1433 | 0.6132 | 0.048* | |
H1WB | 0.6931 | 0.1499 | 0.5112 | 0.048* | |
O2W | 0.6910 (5) | 0.0106 (15) | 0.7359 (8) | 0.065 (3) | |
H2WA | 0.6846 | −0.0992 | 0.7221 | 0.098* | |
H2WB | 0.7077 | 0.0156 | 0.7994 | 0.098* | |
O3W | 0.5418 (4) | 0.0093 (14) | 0.6535 (8) | 0.052 (3) | |
H3WA | 0.5548 | −0.0801 | 0.6239 | 0.078* | |
H3WB | 0.5533 | 0.1042 | 0.6271 | 0.078* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
K1 | 0.061 (2) | 0.0327 (16) | 0.057 (2) | −0.0080 (19) | −0.0005 (15) | 0.0032 (18) |
Nd1 | 0.0132 (3) | 0.0187 (3) | 0.0127 (3) | −0.0015 (3) | 0.00443 (18) | −0.0010 (3) |
O1 | 0.058 (5) | 0.049 (5) | 0.018 (4) | −0.033 (5) | 0.007 (4) | −0.007 (4) |
O2 | 0.048 (5) | 0.063 (6) | 0.019 (4) | −0.044 (5) | 0.008 (4) | −0.004 (4) |
O3 | 0.044 (5) | 0.027 (4) | 0.014 (4) | −0.007 (4) | 0.005 (3) | −0.002 (3) |
O4 | 0.031 (4) | 0.022 (4) | 0.019 (4) | −0.006 (3) | 0.008 (3) | 0.000 (3) |
O5 | 0.013 (3) | 0.017 (4) | 0.021 (4) | 0.004 (3) | 0.005 (3) | −0.001 (3) |
O6 | 0.012 (4) | 0.022 (4) | 0.026 (4) | −0.006 (3) | 0.006 (3) | −0.011 (3) |
O7 | 0.024 (4) | 0.016 (4) | 0.077 (6) | 0.001 (4) | 0.014 (4) | 0.011 (4) |
O8 | 0.014 (4) | 0.018 (4) | 0.036 (4) | −0.001 (3) | 0.003 (3) | −0.001 (3) |
C1 | 0.026 (6) | 0.049 (8) | 0.010 (6) | −0.019 (6) | 0.005 (5) | 0.001 (6) |
C2 | 0.016 (5) | 0.014 (5) | 0.009 (5) | 0.005 (4) | 0.000 (4) | 0.001 (4) |
C3 | 0.023 (6) | 0.016 (6) | 0.009 (6) | −0.002 (5) | 0.007 (5) | −0.002 (4) |
C4 | 0.018 (6) | 0.019 (6) | 0.020 (6) | −0.002 (5) | 0.009 (4) | 0.007 (5) |
O1W | 0.041 (5) | 0.025 (4) | 0.033 (4) | 0.013 (4) | 0.019 (4) | 0.012 (4) |
O2W | 0.086 (7) | 0.053 (6) | 0.051 (6) | 0.004 (6) | −0.009 (5) | 0.001 (5) |
O3W | 0.058 (5) | 0.046 (5) | 0.057 (5) | −0.006 (5) | 0.021 (4) | −0.014 (5) |
Geometric parameters (Å, º) top
Nd1—O1i | 2.492 (8) | O1—C1 | 1.244 (14) |
Nd1—O2 | 2.502 (8) | O2—C1 | 1.264 (14) |
Nd1—O3i | 2.527 (7) | O3—C2 | 1.238 (13) |
Nd1—O4 | 2.514 (8) | O4—C2 | 1.270 (12) |
Nd1—O5 | 2.455 (7) | O5—C3 | 1.240 (13) |
Nd1—O6ii | 2.444 (7) | O6—C3 | 1.245 (13) |
Nd1—O7 | 2.505 (8) | O7—C4 | 1.231 (13) |
Nd1—O8iii | 2.472 (8) | O8—C4 | 1.254 (12) |
Nd1—O1W | 2.432 (8) | C1—C2 | 1.540 (16) |
K1—O1iv | 3.161 (11) | C3—C3ii | 1.59 (2) |
K1—O3 | 2.781 (9) | C4—C4iii | 1.53 (2) |
K1—O5v | 2.936 (8) | O1W—H1WA | 0.85 |
K1—O6vi | 3.377 (9) | O1W—H1WB | 0.85 |
K1—O8vii | 2.857 (8) | O2W—H2WA | 0.85 |
K1—O1Wv | 3.336 (9) | O2W—H2WB | 0.85 |
K1—O2W | 3.324 (13) | O3W—H3WA | 0.85 |
K1—O3W | 2.841 (11) | O3W—H3WB | 0.85 |
K1—O3Wvi | 2.803 (10) | | |
| | | |
O3—K1—O3Wvi | 96.4 (3) | O5—Nd1—O4 | 69.1 (2) |
O3—K1—O3W | 81.1 (3) | O8iii—Nd1—O4 | 132.3 (3) |
O3Wvi—K1—O3W | 73.9 (3) | O1i—Nd1—O4 | 125.5 (3) |
O3—K1—O8vii | 57.9 (2) | O2—Nd1—O4 | 64.3 (3) |
O3Wvi—K1—O8vii | 136.7 (3) | O7—Nd1—O4 | 117.4 (3) |
O3W—K1—O8vii | 127.0 (3) | O1W—Nd1—O3i | 130.4 (3) |
O3—K1—O5v | 163.4 (3) | O6ii—Nd1—O3i | 72.2 (3) |
O3Wvi—K1—O5v | 74.0 (3) | O5—Nd1—O3i | 74.8 (3) |
O3W—K1—O5v | 108.4 (3) | O8iii—Nd1—O3i | 66.1 (3) |
O8vii—K1—O5v | 120.4 (2) | O1i—Nd1—O3i | 64.2 (3) |
O3—K1—O1iv | 133.0 (3) | O2—Nd1—O3i | 130.8 (3) |
O3Wvi—K1—O1iv | 126.7 (3) | O7—Nd1—O3i | 104.3 (3) |
O3W—K1—O1iv | 92.8 (3) | O4—Nd1—O3i | 138.2 (3) |
O8vii—K1—O1iv | 92.7 (2) | C1—O1—Nd1viii | 120.2 (8) |
O5v—K1—O1iv | 61.6 (2) | C1—O1—K1ix | 113.1 (8) |
O3—K1—O2W | 76.2 (3) | Nd1viii—O1—K1ix | 97.6 (3) |
O3Wvi—K1—O2W | 141.1 (3) | C1—O2—Nd1 | 121.2 (7) |
O3W—K1—O2W | 67.3 (3) | C2—O3—Nd1viii | 120.0 (7) |
O8vii—K1—O2W | 71.2 (3) | C2—O3—K1 | 122.6 (7) |
O5v—K1—O2W | 119.8 (3) | Nd1viii—O3—K1 | 107.1 (3) |
O1iv—K1—O2W | 58.9 (3) | C2—O4—Nd1 | 121.4 (7) |
O3—K1—O1Wv | 118.1 (2) | C3—O5—Nd1 | 119.2 (6) |
O3Wvi—K1—O1Wv | 129.6 (3) | C3—O5—K1x | 135.2 (7) |
O3W—K1—O1Wv | 142.2 (3) | Nd1—O5—K1x | 104.6 (2) |
O8vii—K1—O1Wv | 60.3 (2) | C3—O6—Nd1ii | 119.4 (7) |
O5v—K1—O1Wv | 62.7 (2) | C3—O6—K1vi | 122.0 (6) |
O1iv—K1—O1Wv | 49.9 (2) | Nd1ii—O6—K1vi | 93.0 (2) |
O2W—K1—O1Wv | 85.3 (2) | C4—O7—Nd1 | 122.0 (7) |
O3—K1—O6vi | 55.8 (2) | C4—O8—Nd1iii | 122.4 (7) |
O3Wvi—K1—O6vi | 75.4 (3) | C4—O8—K1xi | 126.2 (7) |
O3W—K1—O6vi | 122.6 (3) | Nd1iii—O8—K1xi | 106.3 (3) |
O8vii—K1—O6vi | 61.4 (2) | O1—C1—O2 | 125.7 (12) |
O5v—K1—O6vi | 108.0 (2) | O1—C1—C2 | 117.3 (10) |
O1iv—K1—O6vi | 143.9 (2) | O2—C1—C2 | 117.0 (10) |
O2W—K1—O6vi | 124.8 (2) | O3—C2—O4 | 127.7 (10) |
O1Wv—K1—O6vi | 94.0 (2) | O3—C2—C1 | 116.5 (9) |
O1W—Nd1—O6ii | 137.8 (3) | O4—C2—C1 | 115.7 (9) |
O1W—Nd1—O5 | 84.3 (3) | O5—C3—O6 | 127.1 (10) |
O6ii—Nd1—O5 | 66.7 (2) | O5—C3—C3ii | 116.4 (12) |
O1W—Nd1—O8iii | 137.4 (3) | O6—C3—C3ii | 116.4 (12) |
O6ii—Nd1—O8iii | 81.7 (2) | O7—C4—O8 | 128.0 (10) |
O5—Nd1—O8iii | 135.7 (2) | O7—C4—C4iii | 116.0 (11) |
O1W—Nd1—O1i | 67.8 (3) | O8—C4—C4iii | 115.9 (12) |
O6ii—Nd1—O1i | 129.6 (3) | Nd1—O1W—K1x | 94.4 (3) |
O5—Nd1—O1i | 78.4 (3) | Nd1—O1W—H1WA | 132.1 |
O8iii—Nd1—O1i | 101.6 (3) | K1x—O1W—H1WA | 110.5 |
O1W—Nd1—O2 | 97.6 (3) | Nd1—O1W—H1WB | 117.7 |
O6ii—Nd1—O2 | 79.0 (3) | K1x—O1W—H1WB | 67.2 |
O5—Nd1—O2 | 127.7 (3) | H1WA—O1W—H1WB | 109.7 |
O8iii—Nd1—O2 | 70.9 (3) | K1—O2W—H2WA | 88.2 |
O1i—Nd1—O2 | 150.1 (3) | K1—O2W—H2WB | 75.5 |
O1W—Nd1—O7 | 74.0 (3) | H2WA—O2W—H2WB | 106.4 |
O6ii—Nd1—O7 | 142.0 (2) | K1vi—O3W—K1 | 106.0 (3) |
O5—Nd1—O7 | 150.6 (3) | K1vi—O3W—H3WA | 110.4 |
O8iii—Nd1—O7 | 63.5 (2) | K1—O3W—H3WA | 110.7 |
O1i—Nd1—O7 | 75.1 (3) | K1vi—O3W—H3WB | 110.4 |
O2—Nd1—O7 | 75.7 (3) | K1—O3W—H3WB | 110.6 |
O1W—Nd1—O4 | 66.5 (3) | H3WA—O3W—H3WB | 108.8 |
O6ii—Nd1—O4 | 74.6 (3) | | |
Symmetry codes: (i) x, −y+1, z−1/2; (ii) −x+1, −y+1, −z+1; (iii) −x+3/2, −y+3/2, −z+1; (iv) x, y−1, z; (v) x, −y, z+1/2; (vi) −x+1, y, −z+3/2; (vii) −x+3/2, y−1/2, −z+3/2; (viii) x, −y+1, z+1/2; (ix) x, y+1, z; (x) x, −y, z−1/2; (xi) −x+3/2, y+1/2, −z+3/2. |
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