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Of the three fumarate groups in the title compound, [Tb2(C4H2O4)3(H2O)4]·C3H7NO, one lies on a special position of site symmetry \overline{1}, whereas the other two lie on special positions of site symmetry 2. The three link the water-coordinated Tb atoms to form a layer structure. The water mol­ecules inter­act within each layer, and the disordered N,N-dimethyl­formamide mol­ecules occupy the space between adjacent layers. The Tb atom shows square–anti­prismatic coordination.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807011282/sj2239sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536807011282/sj2239Isup2.hkl
Contains datablock I

CCDC reference: 632024

Key indicators

  • Single-crystal X-ray study
  • T = 295 K
  • Mean [sigma](C-C) = 0.006 Å
  • Disorder in main residue
  • R factor = 0.024
  • wR factor = 0.076
  • Data-to-parameter ratio = 16.5

checkCIF/PLATON results

No syntax errors found



Alert level A PLAT415_ALERT_2_A Short Inter D-H..H-X H1W1 .. H8'C .. 1.86 Ang.
Author Response: ... This is a artifact of not allowing the methyl group to rotate so as to fit the electron density. The methyl groups of the DMF are disordered.

Alert level C PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings Differ .... ? PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT045_ALERT_1_C Calculated and Reported Z Differ by ............ 0.25 Ratio PLAT062_ALERT_4_C Rescale T(min) & T(max) by ..................... 0.85 PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for O5 PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for C7 PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for C7' PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for C8 PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for C8' PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for Tb1 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for O7 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for O7' PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for N1 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for N1' PLAT250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor .... 2.09 PLAT301_ALERT_3_C Main Residue Disorder ......................... 3.00 Perc. PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 10
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: C15 H21 N1 O17 Tb2 Atom count from _chemical_formula_moiety:C15 H21 N2 O17 Tb2 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 0.846 Tmax scaled 0.367 Tmin scaled 0.311
1 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 17 ALERT level C = Check and explain 2 ALERT level G = General alerts; check 4 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 12 ALERT type 2 Indicator that the structure model may be wrong or deficient 2 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: RAPID-AUTO (Rigaku, 1998); cell refinement: RAPID-AUTO; data reduction: CrystalStructure (Rigaku/MSC, 2002); program(s) used to solve structure: atomic coordinates from published structure (Reference?); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: X-SEED (Barbour, 2001); software used to prepare material for publication: publCIF (Westrip, 2007).

Poly[[tetraaquabis(µ4-fumarato-κ4O:O':O'':O''')(µ2-fumarato- κ4O,O':O'',O'''')diterbium(III)] N,N-dimethylformamide solvate] top
Crystal data top
[Tb2(C4H2O4)3(H2O)4]·C3H7NOF(000) = 1536
Mr = 805.17Dx = 1.883 Mg m3
Monoclinic, C2/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2ycCell parameters from 11960 reflections
a = 16.422 (7) Åθ = 3.1–27.5°
b = 18.079 (9) ŵ = 5.01 mm1
c = 9.631 (3) ÅT = 295 K
β = 96.71 (2)°Block, green
V = 2840 (2) Å30.25 × 0.23 × 0.20 mm
Z = 4
Data collection top
Rigaki R-AXIS IP area-detector
diffractometer
3258 independent reflections
Radiation source: fine-focus sealed tube2976 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.019
ω scansθmax = 27.5°, θmin = 3.1°
Absorption correction: multi-scan
(ABSCOR; Higashi, 1995)
h = 2121
Tmin = 0.367, Tmax = 0.434k = 2323
13547 measured reflectionsl = 1112
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)] = 0.024Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.076H-atom parameters constrained
S = 1.07 w = 1/[σ2(Fo2) + (0.0475P)2 + 12.1038P]
where P = (Fo2 + 2Fc2)/3
3258 reflections(Δ/σ)max = 0.001
198 parametersΔρmax = 1.16 e Å3
48 restraintsΔρmin = 0.65 e Å3
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Tb10.249656 (9)0.513399 (10)0.532361 (16)0.01778 (8)
O10.1979 (2)0.39360 (17)0.6023 (3)0.0334 (7)
O20.2915 (2)0.38392 (18)0.4586 (3)0.0334 (7)
O30.17932 (18)0.48211 (16)0.3139 (3)0.0273 (6)
O40.11733 (17)0.4629 (2)0.1016 (3)0.0286 (6)
O50.37118 (18)0.5345 (2)0.4357 (3)0.0374 (8)
O60.3464 (2)0.5227 (2)0.2084 (4)0.0453 (10)
O1W0.2183 (2)0.62429 (19)0.3923 (3)0.0419 (8)
H1W10.18240.64970.42800.050*
H1W20.19980.61200.30940.050*
O2W0.2793 (2)0.6243 (2)0.6683 (3)0.0433 (9)
H2W10.27190.61610.75290.052*
H2W20.24760.65880.63560.052*
C10.2425 (3)0.3550 (3)0.5333 (4)0.0318 (10)
C20.2349 (3)0.2732 (3)0.5425 (5)0.0379 (10)
H20.20710.25380.61300.045*
C30.1155 (2)0.4720 (2)0.2303 (4)0.0202 (7)
C40.0356 (2)0.4703 (2)0.2891 (4)0.0241 (8)
H40.03600.46920.38580.029*
C50.3937 (2)0.5284 (2)0.3161 (4)0.0246 (8)
C60.4842 (2)0.5294 (3)0.3090 (4)0.0302 (9)
H60.51930.53010.39210.036*
O70.1403 (7)0.7579 (6)0.4186 (12)0.0317 (18)0.25
N10.0307 (8)0.7442 (7)0.5318 (15)0.044 (3)0.25
C70.1038 (8)0.7781 (8)0.5176 (15)0.059 (4)0.25
H70.12510.81460.57940.071*0.25
C80.0004 (12)0.6870 (13)0.433 (3)0.070 (6)0.25
H8A0.05170.66880.45730.105*0.25
H8B0.03840.64710.43590.105*0.25
H8C0.00820.70740.34030.105*0.25
C90.0167 (14)0.7637 (14)0.645 (2)0.094 (7)0.25
H9A0.06550.73410.63850.141*0.25
H9B0.03150.81510.63750.141*0.25
H9C0.01550.75490.73290.141*0.25
O7'0.1679 (6)0.7466 (6)0.5943 (12)0.0317 (18)0.25
N1'0.0389 (8)0.7597 (8)0.4712 (14)0.044 (3)0.25
C7'0.1152 (8)0.7872 (8)0.5333 (14)0.059 (4)0.25
H7'0.12580.83750.52790.071*0.25
C8'0.0284 (11)0.6799 (9)0.486 (3)0.070 (6)0.25
H8'A0.02440.66560.44040.105*0.25
H8'B0.03230.66730.58310.105*0.25
H8'C0.07040.65450.44320.105*0.25
C9'0.0173 (12)0.8140 (15)0.403 (2)0.094 (7)0.25
H9'A0.06690.78990.36440.141*0.25
H9'B0.00770.83780.32960.141*0.25
H9'C0.02980.85030.47020.141*0.25
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Tb10.01182 (11)0.02661 (12)0.01545 (11)0.00061 (6)0.00393 (7)0.00092 (6)
O10.0454 (18)0.0274 (15)0.0292 (15)0.0009 (13)0.0118 (13)0.0028 (12)
O20.0436 (18)0.0329 (16)0.0251 (14)0.0081 (14)0.0089 (13)0.0006 (12)
O30.0161 (13)0.0386 (17)0.0262 (15)0.0023 (11)0.0024 (11)0.0021 (12)
O40.0179 (13)0.0502 (17)0.0191 (13)0.0036 (13)0.0083 (10)0.0014 (13)
O50.0206 (14)0.074 (2)0.0196 (14)0.0043 (15)0.0104 (12)0.0011 (15)
O60.0164 (14)0.094 (3)0.0250 (16)0.0059 (16)0.0001 (13)0.0102 (17)
O1W0.069 (2)0.0347 (17)0.0225 (14)0.0067 (16)0.0079 (15)0.0008 (13)
O2W0.066 (2)0.0434 (19)0.0210 (14)0.0169 (17)0.0098 (15)0.0033 (13)
C10.045 (3)0.030 (2)0.0199 (19)0.0055 (18)0.0016 (18)0.0003 (15)
C20.054 (3)0.032 (2)0.030 (2)0.005 (2)0.012 (2)0.0032 (17)
C30.0152 (16)0.0271 (19)0.0191 (17)0.0009 (14)0.0047 (14)0.0011 (14)
C40.0174 (17)0.041 (2)0.0154 (15)0.0006 (16)0.0071 (14)0.0004 (15)
C50.0153 (17)0.037 (2)0.0224 (18)0.0015 (15)0.0053 (14)0.0010 (16)
C60.0146 (17)0.057 (3)0.0194 (18)0.0001 (18)0.0031 (14)0.0031 (19)
O70.027 (4)0.023 (4)0.047 (4)0.001 (3)0.012 (3)0.001 (4)
N10.035 (5)0.041 (7)0.061 (8)0.001 (4)0.022 (6)0.012 (6)
C70.055 (6)0.058 (7)0.071 (7)0.009 (6)0.033 (6)0.009 (6)
C80.069 (10)0.064 (8)0.076 (10)0.005 (7)0.006 (8)0.008 (8)
C90.097 (11)0.094 (11)0.092 (10)0.002 (8)0.017 (8)0.008 (8)
O7'0.027 (4)0.023 (4)0.047 (4)0.001 (3)0.012 (3)0.001 (4)
N1'0.035 (5)0.041 (7)0.061 (8)0.001 (4)0.022 (6)0.012 (6)
C7'0.055 (6)0.058 (7)0.071 (7)0.009 (6)0.033 (6)0.009 (6)
C8'0.069 (10)0.064 (8)0.076 (10)0.005 (7)0.006 (8)0.008 (8)
C9'0.097 (11)0.094 (11)0.092 (10)0.002 (8)0.017 (8)0.008 (8)
Geometric parameters (Å, º) top
Tb1—O12.450 (3)N1'—C7'1.414 (9)
Tb1—O22.564 (3)N1'—C9'1.451 (10)
Tb1—O32.348 (3)N1'—C8'1.461 (10)
Tb1—O4i2.385 (3)O1W—H1W10.85
Tb1—O52.330 (3)O1W—H1W20.85
Tb1—O6i2.280 (3)O2W—H2W10.85
Tb1—O1W2.437 (3)O2W—H2W20.85
Tb1—O2W2.412 (3)C2—H20.9300
O1—C11.256 (5)C4—H40.9300
O2—C11.256 (5)C6—H60.9300
O3—C31.259 (5)C7—H70.9300
O4—C31.254 (5)C8—H8A0.9600
O5—C51.254 (5)C8—H8B0.9600
O6—C51.225 (6)C8—H8C0.9600
C1—C21.487 (7)C9—H9A0.9600
C2—C2ii1.309 (9)C9—H9B0.9600
C3—C41.489 (5)C9—H9C0.9600
C4—C4iii1.314 (8)C7'—H7'0.9300
C5—C61.496 (5)C8'—H8'A0.9600
C6—C6iv1.303 (8)C8'—H8'B0.9600
O7—C71.239 (10)C8'—H8'C0.9600
N1—C71.370 (9)C9'—H9'A0.9600
N1—C81.457 (10)C9'—H9'B0.9600
N1—C91.453 (10)C9'—H9'C0.9600
O7'—C7'1.230 (10)
O1—Tb1—O251.8 (1)C7—N1—C9121.3 (11)
O1—Tb1—O383.3 (1)C8—N1—C9119.0 (15)
O1—Tb1—O4i74.0 (1)O7—C7—N1117.0 (9)
O1—Tb1—O5126.5 (1)C7'—N1'—C9'116.0 (10)
O1—Tb1—O6i77.1 (1)C7'—N1'—C8'114.5 (9)
O1—Tb1—O1W145.3 (1)C9'—N1'—C8'129.5 (14)
O1—Tb1—O2W129.8 (1)O7'—C7'—N1'122.2 (10)
O2—Tb1—O369.6 (1)Tb1—O1W—H1W1109.5
O2—Tb1—O4i121.6 (1)Tb1—O1W—H1W2109.5
O2—Tb1—O576.6 (1)H1W1—O1W—H1W2109.5
O2—Tb1—O6i76.0 (1)Tb1—O2W—H2W1109.5
O2—Tb1—O1W130.1 (1)Tb1—O2W—H2W2109.5
O2—Tb1—O2W149.9 (1)C2ii—C2—H2118.0
O3—Tb1—O4i85.7 (1)C1—C2—H2118.0
O3—Tb1—O592.1 (1)C4iii—C4—H4118.5
O3—Tb1—O6i145.6 (1)C3—C4—H4118.5
O3—Tb1—O1W69.7 (1)C6iv—C6—H6118.7
O3—Tb1—O2W137.2 (1)C5—C6—H6118.7
O4i—Tb1—O5158.9 (2)O7—C7—H7121.5
O4i—Tb1—O6i115.0 (1)N1—C7—H7121.5
O4i—Tb1—O1W82.3 (1)N1—C8—H8A109.5
O4i—Tb1—O2W80.3 (1)N1—C8—H8B109.5
O5—Tb1—O6i77.8 (1)H8A—C8—H8B109.5
O5—Tb1—O1W77.3 (1)N1—C8—H8C109.5
O5—Tb1—O2W87.3 (1)H8A—C8—H8C109.5
O6i—Tb1—O2W75.9 (1)H8B—C8—H8C109.5
O6i—Tb1—O1W137.0 (1)N1—C9—H9A109.5
O1W—Tb1—O2W68.5 (1)N1—C9—H9B109.5
C1—O1—Tb195.9 (3)H9A—C9—H9B109.5
C1—O2—Tb190.6 (3)N1—C9—H9C109.5
C3—O3—Tb1153.4 (3)H9A—C9—H9C109.5
C3—O4—Tb1v112.4 (2)H9B—C9—H9C109.5
C5—O5—Tb1135.3 (3)O7'—C7'—H7'118.9
C5—O6—Tb1v166.2 (4)N1'—C7'—H7'118.9
O2—C1—O1121.6 (4)N1'—C8'—H8'A109.5
O2—C1—C2120.8 (4)N1'—C8'—H8'B109.5
O1—C1—C2117.6 (4)H8'A—C8'—H8'B109.5
C2ii—C2—C1124.1 (6)N1'—C8'—H8'C109.5
O4—C3—O3122.5 (3)H8'A—C8'—H8'C109.5
O4—C3—C4119.8 (3)H8'B—C8'—H8'C109.5
O3—C3—C4117.7 (3)N1'—C9'—H9'A109.5
C4iii—C4—C3123.0 (4)N1'—C9'—H9'B109.5
O6—C5—O5124.0 (4)H9'A—C9'—H9'B109.5
O6—C5—C6119.8 (4)N1'—C9'—H9'C109.5
O5—C5—C6116.2 (4)H9'A—C9'—H9'C109.5
C6iv—C6—C5122.6 (5)H9'B—C9'—H9'C109.5
C7—N1—C8119.7 (10)
O6i—Tb1—O1—C181.6 (3)O1—Tb1—O5—C579.9 (5)
O5—Tb1—O1—C117.7 (3)O2—Tb1—O5—C565.2 (5)
O3—Tb1—O1—C169.9 (3)Tb1—O2—C1—O11.1 (4)
O4i—Tb1—O1—C1157.3 (3)Tb1—O2—C1—C2179.2 (4)
O2W—Tb1—O1—C1140.5 (3)Tb1—O1—C1—O21.2 (4)
O1W—Tb1—O1—C1108.3 (3)Tb1—O1—C1—C2179.1 (3)
O2—Tb1—O1—C10.6 (2)O2—C1—C2—C2ii13.3 (9)
O6i—Tb1—O2—C183.8 (3)O1—C1—C2—C2ii166.4 (6)
O5—Tb1—O2—C1164.3 (3)Tb1v—O4—C3—O39.4 (5)
O3—Tb1—O2—C198.3 (3)Tb1v—O4—C3—C4171.2 (3)
O4i—Tb1—O2—C127.2 (3)Tb1—O3—C3—O4169.1 (4)
O2W—Tb1—O2—C1104.8 (3)Tb1—O3—C3—C411.5 (8)
O1W—Tb1—O2—C1135.4 (2)O4—C3—C4—C4iii10.1 (5)
O1—Tb1—O2—C10.6 (2)O3—C3—C4—C4iii170.4 (2)
O6i—Tb1—O3—C3127.3 (6)Tb1v—O6—C5—O562.9 (16)
O5—Tb1—O3—C3161.5 (6)Tb1v—O6—C5—C6118.1 (12)
O4i—Tb1—O3—C32.4 (6)Tb1—O5—C5—O616.4 (8)
O2W—Tb1—O3—C373.2 (6)Tb1—O5—C5—C6164.5 (3)
O1W—Tb1—O3—C385.8 (6)O6—C5—C6—C6iv4.6 (6)
O1—Tb1—O3—C372.0 (6)O5—C5—C6—C6iv174.5 (3)
O2—Tb1—O3—C3123.6 (6)C9—N1—C7—O7179.8 (3)
O6i—Tb1—O5—C5143.5 (5)C8—N1—C7—O70.2 (3)
O3—Tb1—O5—C53.3 (5)C7—N1—C9—C9vi55.8 (15)
O4i—Tb1—O5—C586.6 (6)C8—N1—C9—C9vi123.8 (15)
O2W—Tb1—O5—C5140.4 (5)C9'—N1'—C7'—O7'179.9 (3)
O1W—Tb1—O5—C571.9 (5)C8'—N1'—C7'—O7'0.1 (3)
Symmetry codes: (i) x, y+1, z+1/2; (ii) x+1/2, y+1/2, z+1; (iii) x, y, z+1/2; (iv) x+1, y, z+1/2; (v) x, y+1, z1/2; (vi) x, y, z+3/2.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1W—H1W1···O70.852.072.76 (1)137
O1W—H1W2···O1v0.851.992.793 (4)156
O2W—H2W1···O2i0.851.972.783 (4)160
O2W—H2W2···O70.852.072.91 (1)169
Symmetry codes: (i) x, y+1, z+1/2; (v) x, y+1, z1/2.
 

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