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The title compound, [Gd2(C8H22N2O12P4)(C2O4)2(H2O)2]·4H2O, was synthesized by the hydro­thermal method. It exhibits a pillar–layer structure, with the layers formed by GdIII ions inter­connected by the oxalate ions and the –NH(CH2PO3H)2 units of the tetra­phospho­nate dianions. The central organic groups of the tetra­phospho­nate ligands act as the pillars. Each oxalate ion bridges two GdIII ions and each tetra­phospho­nate ligand bridges six GdIII ions. Inversion centres are located at the mid-points of the central C—C bonds of both types of ligands.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807000049/sa2032sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536807000049/sa2032Isup2.hkl
Contains datablock I

CCDC reference: 636792

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](C-C) = 0.013 Å
  • R factor = 0.045
  • wR factor = 0.101
  • Data-to-parameter ratio = 12.4

checkCIF/PLATON results

No syntax errors found



Alert level B PLAT222_ALERT_3_B Large Non-Solvent H Ueq(max)/Ueq(min) ... 5.00 Ratio
Alert level C PLAT048_ALERT_1_C MoietyFormula Not Given ........................ ? PLAT062_ALERT_4_C Rescale T(min) & T(max) by ..................... 0.98 PLAT152_ALERT_1_C Supplied and Calc Volume s.u. Inconsistent ..... ? PLAT153_ALERT_1_C The su's on the Cell Axes are Equal (x 100000) . 60 Ang. PLAT213_ALERT_2_C Atom N1 has ADP max/min Ratio ............. 3.60 oblat PLAT250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor .... 2.74 PLAT342_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 13 PLAT417_ALERT_2_C Short Inter D-H..H-D H4 .. H12A .. 2.11 Ang. PLAT764_ALERT_4_C Overcomplete CIF Bond List Detected (Rep/Expd) . 1.15 Ratio
Alert level G PLAT199_ALERT_1_G Check the Reported _cell_measurement_temperature 293 K PLAT200_ALERT_1_G Check the Reported _diffrn_ambient_temperature . 293 K
0 ALERT level A = In general: serious problem 1 ALERT level B = Potentially serious problem 9 ALERT level C = Check and explain 2 ALERT level G = General alerts; check 5 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 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: APEX2 (Bruker, 2004); cell refinement: SMART (Bruker, 2004); data reduction: SAINT (Bruker, 2004); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 (Farrugia, 1997); software used to prepare material for publication: SHELXL97.

catena Poly[diaqua bis(oxalic acid) (tetramethylphosphono-1,4-diaminobutane) digadolinium(III)] tetrahydrate top
Crystal data top
[Gd2(C2O4)2(C8H22O12N2P4)(H2O)2]·4H2OZ = 2
Mr = 530.40F(000) = 516
Triclinic, P1Dx = 2.305 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 9.5191 (6) ÅCell parameters from 2718 reflections
b = 9.6282 (6) Åθ = 2.3–24.7°
c = 9.6452 (6) ŵ = 4.62 mm1
α = 106.939 (3)°T = 293 K
β = 98.292 (3)°Needle, colourless
γ = 110.123 (2)°0.25 × 0.04 × 0.03 mm
V = 764.05 (8) Å3
Data collection top
Bruker SMART CCD area-detector
diffractometer
2728 independent reflections
Radiation source: fine-focus sealed tube2140 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.048
ω scansθmax = 25.2°, θmin = 2.3°
Absorption correction: multi-scan
(SADABS; Sheldrick, 2003)
h = 1111
Tmin = 0.387, Tmax = 0.893k = 1111
6629 measured reflectionsl = 1111
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.045H atoms treated by a mixture of independent and constrained refinement
wR(F2) = 0.101 w = 1/[σ2(Fo2) + (0.0597P)2]
where P = (Fo2 + 2Fc2)/3
S = 0.94(Δ/σ)max = 0.001
2728 reflectionsΔρmax = 1.78 e Å3
220 parametersΔρmin = 1.92 e Å3
15 restraintsExtinction correction: SHELXL (Sheldrick, 1997)
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.0049 (8)
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
Gd10.58737 (5)0.72593 (4)0.81782 (4)0.02119 (15)
P10.2630 (3)0.4901 (2)0.4847 (2)0.0234 (5)
P20.2393 (3)0.9714 (2)0.3473 (3)0.0297 (5)
N10.2567 (9)0.6690 (8)0.3055 (8)0.0276 (18)
H1A0.312 (9)0.625 (9)0.276 (8)0.02 (2)*
O70.4647 (7)0.6667 (6)1.0071 (6)0.0338 (14)
O80.6016 (7)1.1558 (6)1.1714 (6)0.0307 (13)
O90.4134 (7)0.5155 (6)1.1446 (6)0.0308 (14)
O100.6749 (6)0.9783 (6)1.0313 (6)0.0303 (14)
O10.0893 (6)0.3920 (6)0.4747 (7)0.0363 (15)
H10.05250.31060.39910.054*
O20.3090 (6)0.4033 (6)0.3569 (6)0.0258 (13)
O30.3573 (6)0.5350 (6)0.6421 (6)0.0261 (13)
O60.0686 (7)0.9018 (7)0.2696 (8)0.0473 (17)
O50.3374 (7)1.1078 (6)0.3124 (7)0.0377 (15)
O40.2726 (8)1.0112 (7)0.5199 (7)0.0459 (18)
H40.25061.08600.55880.069*
O130.8584 (8)0.7984 (8)0.9529 (8)0.0448 (16)
H13B0.91710.83360.90530.067*
H13A0.888 (14)0.822 (14)1.047 (4)0.10 (5)*
O120.7750 (9)0.7605 (8)0.2989 (7)0.0503 (18)
H12B0.77050.68480.33060.07 (4)*
H12A0.87090.81110.30770.08 (4)*
O110.0404 (7)0.8710 (7)0.7654 (7)0.0463 (17)
H11B0.13280.91180.82410.08 (4)*
H11A0.02170.94230.74250.09 (5)*
C10.0787 (11)0.5600 (10)0.0478 (10)0.045 (3)
H120.09440.66280.04170.054*
H110.15760.52910.01180.054*
C20.0938 (10)0.5714 (9)0.2129 (9)0.035 (2)
H220.02660.61880.25370.042*
H210.06070.46560.21640.042*
C30.3293 (10)0.8288 (9)0.2943 (10)0.030 (2)
H320.33320.81140.19090.036*
H310.43590.87960.35640.036*
C40.2774 (11)0.6785 (9)0.4664 (9)0.032 (2)
H420.19850.70730.50480.038*
H410.37830.76140.52730.038*
C50.5786 (9)1.0380 (8)1.0576 (9)0.0257 (19)
C60.4646 (9)0.5530 (9)1.0430 (9)0.0215 (18)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Gd10.0333 (3)0.0148 (2)0.0241 (3)0.01659 (17)0.01083 (18)0.00941 (17)
P10.0332 (13)0.0179 (10)0.0264 (12)0.0159 (9)0.0105 (10)0.0103 (9)
P20.0417 (15)0.0219 (11)0.0392 (14)0.0205 (10)0.0179 (12)0.0178 (10)
N10.047 (5)0.019 (4)0.033 (4)0.027 (4)0.017 (4)0.013 (3)
O70.052 (4)0.028 (3)0.041 (4)0.029 (3)0.020 (3)0.021 (3)
O80.040 (4)0.026 (3)0.029 (3)0.020 (3)0.004 (3)0.007 (3)
O90.049 (4)0.028 (3)0.040 (4)0.030 (3)0.026 (3)0.022 (3)
O100.034 (3)0.023 (3)0.035 (4)0.023 (3)0.005 (3)0.002 (3)
O10.035 (4)0.029 (3)0.043 (4)0.013 (3)0.018 (3)0.007 (3)
O20.040 (4)0.026 (3)0.026 (3)0.023 (3)0.018 (3)0.014 (3)
O30.036 (3)0.015 (3)0.028 (3)0.014 (2)0.004 (3)0.006 (2)
O60.042 (4)0.031 (3)0.077 (5)0.023 (3)0.018 (4)0.022 (3)
O50.055 (4)0.024 (3)0.049 (4)0.022 (3)0.025 (3)0.024 (3)
O40.086 (5)0.035 (4)0.044 (4)0.046 (4)0.032 (4)0.019 (3)
O130.049 (4)0.046 (4)0.040 (5)0.029 (3)0.010 (4)0.006 (3)
O120.066 (6)0.040 (4)0.057 (5)0.026 (4)0.026 (4)0.025 (4)
O110.037 (4)0.035 (4)0.053 (5)0.013 (3)0.005 (4)0.007 (3)
C10.059 (7)0.038 (5)0.040 (6)0.022 (5)0.003 (5)0.019 (5)
C20.048 (6)0.021 (4)0.034 (5)0.018 (4)0.001 (5)0.010 (4)
C30.039 (5)0.024 (4)0.040 (5)0.018 (4)0.017 (4)0.020 (4)
C40.053 (6)0.024 (4)0.018 (5)0.017 (4)0.002 (4)0.010 (4)
C50.035 (5)0.011 (4)0.035 (5)0.014 (4)0.012 (4)0.006 (4)
C60.029 (5)0.018 (4)0.024 (5)0.015 (4)0.008 (4)0.010 (4)
Geometric parameters (Å, º) top
Gd1—O5i2.301 (5)O9—Gd1iv2.452 (5)
Gd1—O32.322 (5)O10—C51.257 (9)
Gd1—O2ii2.337 (5)O1—H10.8200
Gd1—O72.406 (5)O2—Gd1ii2.337 (5)
Gd1—O8iii2.437 (5)O5—Gd1i2.301 (5)
Gd1—O9iv2.452 (5)O4—H40.8200
Gd1—O102.456 (5)O13—H13B0.8200
Gd1—O132.470 (7)O13—H13A0.85 (2)
P1—O21.489 (5)O12—H12B0.8595
P1—O31.501 (5)O12—H12A0.8517
P1—O11.569 (6)O11—H11B0.8590
P1—C41.834 (8)O11—H11A0.8447
P2—O51.488 (5)C1—C1v1.490 (17)
P2—O61.503 (7)C1—C21.546 (11)
P2—O41.553 (6)C1—H120.9700
P2—C31.846 (8)C1—H110.9700
N1—C21.482 (11)C2—H220.9700
N1—C31.498 (9)C2—H210.9700
N1—C41.508 (10)C3—H320.9700
N1—H1A0.82 (8)C3—H310.9700
O7—C61.240 (9)C4—H420.9700
O8—C51.254 (9)C4—H410.9700
O8—Gd1iii2.437 (5)C5—C5iii1.517 (16)
O9—C61.246 (9)C6—C6iv1.524 (14)
O5i—Gd1—O398.9 (2)C4—N1—H1A103 (5)
O5i—Gd1—O2ii76.27 (18)C6—O7—Gd1120.5 (5)
O3—Gd1—O2ii80.85 (19)C5—O8—Gd1iii119.6 (5)
O5i—Gd1—O7148.5 (2)C6—O9—Gd1iv120.2 (5)
O3—Gd1—O786.62 (19)C5—O10—Gd1118.5 (5)
O2ii—Gd1—O7135.15 (17)P1—O1—H1109.5
O5i—Gd1—O8iii78.21 (19)P1—O2—Gd1ii171.8 (3)
O3—Gd1—O8iii73.57 (18)P1—O3—Gd1141.1 (3)
O2ii—Gd1—O8iii140.25 (18)P2—O5—Gd1i159.0 (4)
O7—Gd1—O8iii73.66 (18)P2—O4—H4109.5
O5i—Gd1—O9iv145.7 (2)Gd1—O13—H13B109.5
O3—Gd1—O9iv79.08 (18)Gd1—O13—H13A123 (9)
O2ii—Gd1—O9iv69.60 (17)H13B—O13—H13A122.3
O7—Gd1—O9iv65.78 (18)H12B—O12—H12A105.7
O8iii—Gd1—O9iv131.85 (19)H11B—O11—H11A109.4
O5i—Gd1—O1082.8 (2)C1v—C1—C2109.4 (10)
O3—Gd1—O10138.43 (18)C1v—C1—H12109.8
O2ii—Gd1—O10138.35 (19)C2—C1—H12109.8
O7—Gd1—O1073.11 (19)C1v—C1—H11109.8
O8iii—Gd1—O1066.11 (18)C2—C1—H11109.8
O9iv—Gd1—O10121.41 (18)H12—C1—H11108.2
O5i—Gd1—O1392.9 (2)N1—C2—C1110.5 (7)
O3—Gd1—O13148.7 (2)N1—C2—H22109.5
O2ii—Gd1—O1373.9 (2)C1—C2—H22109.5
O7—Gd1—O1398.3 (2)N1—C2—H21109.5
O8iii—Gd1—O13137.6 (2)C1—C2—H21109.5
O9iv—Gd1—O1375.0 (2)H22—C2—H21108.1
O10—Gd1—O1371.68 (19)N1—C3—P2119.1 (6)
O2—P1—O3118.3 (3)N1—C3—H32107.6
O2—P1—O1110.0 (3)P2—C3—H32107.6
O3—P1—O1107.2 (3)N1—C3—H31107.6
O2—P1—C4107.7 (3)P2—C3—H31107.6
O3—P1—C4105.3 (3)H32—C3—H31107.0
O1—P1—C4107.9 (4)N1—C4—P1112.3 (5)
O5—P2—O6115.2 (4)N1—C4—H42109.1
O5—P2—O4111.2 (3)P1—C4—H42109.1
O6—P2—O4112.6 (4)N1—C4—H41109.1
O5—P2—C3102.7 (3)P1—C4—H41109.1
O6—P2—C3113.1 (4)H42—C4—H41107.9
O4—P2—C3100.6 (4)O8—C5—O10125.4 (8)
C2—N1—C3115.1 (6)O8—C5—C5iii117.0 (9)
C2—N1—C4112.2 (7)O10—C5—C5iii117.5 (9)
C3—N1—C4112.4 (6)O7—C6—O9126.7 (7)
C2—N1—H1A110 (5)O7—C6—C6iv118.0 (8)
C3—N1—H1A103 (5)O9—C6—C6iv115.2 (8)
Symmetry codes: (i) x+1, y+2, z+1; (ii) x+1, y+1, z+1; (iii) x+1, y+2, z+2; (iv) x+1, y+1, z+2; (v) x, y+1, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1—H1···O11vi0.821.812.628 (8)177
O13—H13B···O11vii0.821.942.751 (10)168
O4—H4···O12i0.821.812.602 (8)161
O11—H11B···O10iii0.861.872.720 (8)172
O12—H12A···O6vii0.851.922.752 (10)165
O11—H11A···O6viii0.841.992.805 (9)161
Symmetry codes: (i) x+1, y+2, z+1; (iii) x+1, y+2, z+2; (vi) x, y+1, z+1; (vii) x+1, y, z; (viii) x, y+2, z+1.
 

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