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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

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806055231/bi2114sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536806055231/bi2114Isup2.hkl
Contains datablock I

CCDC reference: 636136

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](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

Computing details top

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)]·2H2OF(000) = 1576
Mr = 413.43Dx = 2.487 Mg m3
Monoclinic, C2/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2ycCell parameters from 250 reflections
a = 23.085 (5) Åθ = 2.5–25°
b = 7.4913 (15) ŵ = 5.13 mm1
c = 12.941 (3) ÅT = 293 K
β = 99.286 (3)°Block, pink
V = 2208.6 (8) Å30.26 × 0.13 × 0.11 mm
Z = 8
Data collection top
Rigaku R-AXIS-IV
diffractometer
1985 independent reflections
Radiation source: fine-focus sealed tube1531 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.041
ω scansθmax = 25.3°, θmin = 3.2°
Absorption correction: multi-scan
(ABSCOR; Higashi, 1995)
h = 2719
Tmin = 0.330, Tmax = 0.569k = 88
5056 measured reflectionsl = 1515
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.054Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.120H-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 parametersΔρmax = 0.87 e Å3
66 restraintsΔρmin = 2.08 e Å3
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
xyzUiso*/Ueq
K10.58112 (15)0.0002 (5)0.8731 (3)0.0514 (8)
Nd10.63733 (2)0.50022 (9)0.51386 (4)0.0146 (2)
O10.6605 (4)0.6607 (13)0.8570 (6)0.041 (2)
O20.6703 (4)0.6413 (14)0.6886 (6)0.043 (2)
O30.5968 (4)0.3623 (11)0.8388 (6)0.0281 (19)
O40.5991 (3)0.3587 (10)0.6656 (6)0.0237 (18)
O50.5450 (3)0.3412 (10)0.4542 (5)0.0166 (16)
O60.4498 (3)0.3272 (10)0.4646 (6)0.0197 (17)
O70.7464 (4)0.5266 (11)0.5259 (8)0.039 (2)
O80.8239 (3)0.6983 (10)0.5122 (6)0.0228 (18)
C10.6510 (5)0.5883 (18)0.7694 (8)0.028 (3)
C20.6122 (5)0.4200 (14)0.7579 (8)0.013 (2)
C30.4985 (5)0.4023 (14)0.4762 (7)0.016 (2)
C40.7703 (4)0.6689 (15)0.5105 (8)0.019 (2)
O1W0.6766 (4)0.2032 (11)0.5566 (7)0.032 (2)
H1WA0.68140.14330.61320.048*
H1WB0.69310.14990.51120.048*
O2W0.6910 (5)0.0106 (15)0.7359 (8)0.065 (3)
H2WA0.68460.09920.72210.098*
H2WB0.70770.01560.79940.098*
O3W0.5418 (4)0.0093 (14)0.6535 (8)0.052 (3)
H3WA0.55480.08010.62390.078*
H3WB0.55330.10420.62710.078*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
K10.061 (2)0.0327 (16)0.057 (2)0.0080 (19)0.0005 (15)0.0032 (18)
Nd10.0132 (3)0.0187 (3)0.0127 (3)0.0015 (3)0.00443 (18)0.0010 (3)
O10.058 (5)0.049 (5)0.018 (4)0.033 (5)0.007 (4)0.007 (4)
O20.048 (5)0.063 (6)0.019 (4)0.044 (5)0.008 (4)0.004 (4)
O30.044 (5)0.027 (4)0.014 (4)0.007 (4)0.005 (3)0.002 (3)
O40.031 (4)0.022 (4)0.019 (4)0.006 (3)0.008 (3)0.000 (3)
O50.013 (3)0.017 (4)0.021 (4)0.004 (3)0.005 (3)0.001 (3)
O60.012 (4)0.022 (4)0.026 (4)0.006 (3)0.006 (3)0.011 (3)
O70.024 (4)0.016 (4)0.077 (6)0.001 (4)0.014 (4)0.011 (4)
O80.014 (4)0.018 (4)0.036 (4)0.001 (3)0.003 (3)0.001 (3)
C10.026 (6)0.049 (8)0.010 (6)0.019 (6)0.005 (5)0.001 (6)
C20.016 (5)0.014 (5)0.009 (5)0.005 (4)0.000 (4)0.001 (4)
C30.023 (6)0.016 (6)0.009 (6)0.002 (5)0.007 (5)0.002 (4)
C40.018 (6)0.019 (6)0.020 (6)0.002 (5)0.009 (4)0.007 (5)
O1W0.041 (5)0.025 (4)0.033 (4)0.013 (4)0.019 (4)0.012 (4)
O2W0.086 (7)0.053 (6)0.051 (6)0.004 (6)0.009 (5)0.001 (5)
O3W0.058 (5)0.046 (5)0.057 (5)0.006 (5)0.021 (4)0.014 (5)
Geometric parameters (Å, º) top
Nd1—O1i2.492 (8)O1—C11.244 (14)
Nd1—O22.502 (8)O2—C11.264 (14)
Nd1—O3i2.527 (7)O3—C21.238 (13)
Nd1—O42.514 (8)O4—C21.270 (12)
Nd1—O52.455 (7)O5—C31.240 (13)
Nd1—O6ii2.444 (7)O6—C31.245 (13)
Nd1—O72.505 (8)O7—C41.231 (13)
Nd1—O8iii2.472 (8)O8—C41.254 (12)
Nd1—O1W2.432 (8)C1—C21.540 (16)
K1—O1iv3.161 (11)C3—C3ii1.59 (2)
K1—O32.781 (9)C4—C4iii1.53 (2)
K1—O5v2.936 (8)O1W—H1WA0.85
K1—O6vi3.377 (9)O1W—H1WB0.85
K1—O8vii2.857 (8)O2W—H2WA0.85
K1—O1Wv3.336 (9)O2W—H2WB0.85
K1—O2W3.324 (13)O3W—H3WA0.85
K1—O3W2.841 (11)O3W—H3WB0.85
K1—O3Wvi2.803 (10)
O3—K1—O3Wvi96.4 (3)O5—Nd1—O469.1 (2)
O3—K1—O3W81.1 (3)O8iii—Nd1—O4132.3 (3)
O3Wvi—K1—O3W73.9 (3)O1i—Nd1—O4125.5 (3)
O3—K1—O8vii57.9 (2)O2—Nd1—O464.3 (3)
O3Wvi—K1—O8vii136.7 (3)O7—Nd1—O4117.4 (3)
O3W—K1—O8vii127.0 (3)O1W—Nd1—O3i130.4 (3)
O3—K1—O5v163.4 (3)O6ii—Nd1—O3i72.2 (3)
O3Wvi—K1—O5v74.0 (3)O5—Nd1—O3i74.8 (3)
O3W—K1—O5v108.4 (3)O8iii—Nd1—O3i66.1 (3)
O8vii—K1—O5v120.4 (2)O1i—Nd1—O3i64.2 (3)
O3—K1—O1iv133.0 (3)O2—Nd1—O3i130.8 (3)
O3Wvi—K1—O1iv126.7 (3)O7—Nd1—O3i104.3 (3)
O3W—K1—O1iv92.8 (3)O4—Nd1—O3i138.2 (3)
O8vii—K1—O1iv92.7 (2)C1—O1—Nd1viii120.2 (8)
O5v—K1—O1iv61.6 (2)C1—O1—K1ix113.1 (8)
O3—K1—O2W76.2 (3)Nd1viii—O1—K1ix97.6 (3)
O3Wvi—K1—O2W141.1 (3)C1—O2—Nd1121.2 (7)
O3W—K1—O2W67.3 (3)C2—O3—Nd1viii120.0 (7)
O8vii—K1—O2W71.2 (3)C2—O3—K1122.6 (7)
O5v—K1—O2W119.8 (3)Nd1viii—O3—K1107.1 (3)
O1iv—K1—O2W58.9 (3)C2—O4—Nd1121.4 (7)
O3—K1—O1Wv118.1 (2)C3—O5—Nd1119.2 (6)
O3Wvi—K1—O1Wv129.6 (3)C3—O5—K1x135.2 (7)
O3W—K1—O1Wv142.2 (3)Nd1—O5—K1x104.6 (2)
O8vii—K1—O1Wv60.3 (2)C3—O6—Nd1ii119.4 (7)
O5v—K1—O1Wv62.7 (2)C3—O6—K1vi122.0 (6)
O1iv—K1—O1Wv49.9 (2)Nd1ii—O6—K1vi93.0 (2)
O2W—K1—O1Wv85.3 (2)C4—O7—Nd1122.0 (7)
O3—K1—O6vi55.8 (2)C4—O8—Nd1iii122.4 (7)
O3Wvi—K1—O6vi75.4 (3)C4—O8—K1xi126.2 (7)
O3W—K1—O6vi122.6 (3)Nd1iii—O8—K1xi106.3 (3)
O8vii—K1—O6vi61.4 (2)O1—C1—O2125.7 (12)
O5v—K1—O6vi108.0 (2)O1—C1—C2117.3 (10)
O1iv—K1—O6vi143.9 (2)O2—C1—C2117.0 (10)
O2W—K1—O6vi124.8 (2)O3—C2—O4127.7 (10)
O1Wv—K1—O6vi94.0 (2)O3—C2—C1116.5 (9)
O1W—Nd1—O6ii137.8 (3)O4—C2—C1115.7 (9)
O1W—Nd1—O584.3 (3)O5—C3—O6127.1 (10)
O6ii—Nd1—O566.7 (2)O5—C3—C3ii116.4 (12)
O1W—Nd1—O8iii137.4 (3)O6—C3—C3ii116.4 (12)
O6ii—Nd1—O8iii81.7 (2)O7—C4—O8128.0 (10)
O5—Nd1—O8iii135.7 (2)O7—C4—C4iii116.0 (11)
O1W—Nd1—O1i67.8 (3)O8—C4—C4iii115.9 (12)
O6ii—Nd1—O1i129.6 (3)Nd1—O1W—K1x94.4 (3)
O5—Nd1—O1i78.4 (3)Nd1—O1W—H1WA132.1
O8iii—Nd1—O1i101.6 (3)K1x—O1W—H1WA110.5
O1W—Nd1—O297.6 (3)Nd1—O1W—H1WB117.7
O6ii—Nd1—O279.0 (3)K1x—O1W—H1WB67.2
O5—Nd1—O2127.7 (3)H1WA—O1W—H1WB109.7
O8iii—Nd1—O270.9 (3)K1—O2W—H2WA88.2
O1i—Nd1—O2150.1 (3)K1—O2W—H2WB75.5
O1W—Nd1—O774.0 (3)H2WA—O2W—H2WB106.4
O6ii—Nd1—O7142.0 (2)K1vi—O3W—K1106.0 (3)
O5—Nd1—O7150.6 (3)K1vi—O3W—H3WA110.4
O8iii—Nd1—O763.5 (2)K1—O3W—H3WA110.7
O1i—Nd1—O775.1 (3)K1vi—O3W—H3WB110.4
O2—Nd1—O775.7 (3)K1—O3W—H3WB110.6
O1W—Nd1—O466.5 (3)H3WA—O3W—H3WB108.8
O6ii—Nd1—O474.6 (3)
Symmetry codes: (i) x, y+1, z1/2; (ii) x+1, y+1, z+1; (iii) x+3/2, y+3/2, z+1; (iv) x, y1, z; (v) x, y, z+1/2; (vi) x+1, y, z+3/2; (vii) x+3/2, y1/2, z+3/2; (viii) x, y+1, z+1/2; (ix) x, y+1, z; (x) x, y, z1/2; (xi) x+3/2, y+1/2, z+3/2.
 

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