The crystal structure of the title complex is composed of NdIII cations, citrate trianions and water molecules, and is formulated as [Nd(C6H5O7)(H2O)]n, isostructural with the lanthanum analogue [Baggio & Perec (2004). Inorg. Chem. 43, 6965–6968].
Supporting information
CCDC reference: 262257
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (C-C) = 0.017 Å
- R factor = 0.046
- wR factor = 0.109
- Data-to-parameter ratio = 11.1
checkCIF/PLATON results
No syntax errors found
Alert level C
PLAT029_ALERT_3_C _diffrn_measured_fraction_theta_full Low ....... 0.97
PLAT213_ALERT_2_C Atom O7 has ADP max/min Ratio ............. 3.80 prolat
PLAT342_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 17
0 ALERT level A = In general: serious problem
0 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
2 ALERT type 3 Indicator that the structure quality may be low
0 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: SMART (Siemens, 1996); cell refinement: SMART; data reduction: SAINT (Siemens, 1994); program(s) used to solve structure: SHELXTL (Siemens, 1994); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXL97 (Sheldrick, 1997); software used to prepare material for publication: SHELXL97.
Poly[[aquaneodymiun(III)]-µ
5-citrato]
top
Crystal data top
[Nd(C6H5O7)(H2O)] | F(000) = 1336 |
Mr = 351.36 | Dx = 2.662 Mg m−3 |
Monoclinic, C2/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -C 2yc | Cell parameters from 1574 reflections |
a = 16.6409 (11) Å | θ = 2.7–25.0° |
b = 8.7622 (6) Å | µ = 5.95 mm−1 |
c = 13.9279 (9) Å | T = 293 K |
β = 120.288 (2)° | Prism, colourless |
V = 1753.6 (2) Å3 | 0.25 × 0.19 × 0.18 mm |
Z = 8 | |
Data collection top
Siemens SMART CCD area-detector diffractometer | 1507 independent reflections |
Radiation source: fine-focus sealed tube | 1288 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.033 |
ω scans | θmax = 25.0°, θmin = 2.7° |
Absorption correction: empirical (using intensity measurements) (SADABS; Sheldrick, 1996) | h = −19→16 |
Tmin = 0.245, Tmax = 0.343 | k = −9→10 |
2359 measured reflections | l = −16→14 |
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)] = 0.046 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.109 | H-atom parameters constrained |
S = 1.16 | w = 1/[σ2(Fo2) + (0.0111P)2 + 116.7406P] where P = (Fo2 + 2Fc2)/3 |
1507 reflections | (Δ/σ)max < 0.001 |
136 parameters | Δρmax = 1.31 e Å−3 |
0 restraints | Δρmin = −1.32 e Å−3 |
Special details top
Experimental. empirical from equivalent reflections (XEMP in SHELXTL; Siemens,
1994) |
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 | |
Nd1 | 0.08599 (4) | 0.08142 (7) | 0.17213 (4) | 0.0124 (2) | |
O1 | 0.0839 (5) | −0.0369 (9) | 0.0044 (6) | 0.0190 (17) | |
C1 | 0.1277 (8) | −0.0397 (12) | −0.0462 (8) | 0.013 (2) | |
O2 | 0.0849 (5) | −0.0752 (9) | −0.1490 (6) | 0.0171 (16) | |
C2 | 0.2302 (8) | −0.0034 (14) | 0.0084 (9) | 0.017 (2) | |
H2A | 0.2389 | 0.0739 | −0.0353 | 0.020* | |
H2B | 0.2629 | −0.0944 | 0.0074 | 0.020* | |
O3 | 0.2319 (5) | −0.0725 (9) | 0.2524 (6) | 0.0170 (16) | |
C3 | 0.2746 (7) | 0.0538 (11) | 0.1297 (8) | 0.011 (2) | |
O4 | 0.3276 (5) | −0.1922 (9) | 0.2091 (6) | 0.0167 (17) | |
C4 | 0.3703 (7) | 0.1181 (13) | 0.1703 (9) | 0.017 (2) | |
H4A | 0.3664 | 0.1979 | 0.1199 | 0.020* | |
H4B | 0.4101 | 0.0381 | 0.1693 | 0.020* | |
O5 | 0.4181 (7) | 0.0983 (10) | 0.3617 (7) | 0.035 (2) | |
C5 | 0.4143 (8) | 0.1838 (14) | 0.2881 (10) | 0.023 (3) | |
O6 | 0.4438 (6) | 0.3198 (9) | 0.3059 (7) | 0.0251 (19) | |
C6 | 0.2800 (7) | −0.0813 (13) | 0.2050 (8) | 0.014 (2) | |
O7 | 0.2125 (5) | 0.1700 (9) | 0.1295 (6) | 0.0152 (16) | |
H7 | 0.2431 | 0.2398 | 0.1712 | 0.018* | |
O8 | 0.0161 (6) | 0.3168 (9) | 0.0731 (6) | 0.029 (2) | |
H8A | 0.0045 | 0.3088 | 0.0065 | 0.035* | |
H8B | 0.0537 | 0.3902 | 0.1049 | 0.035* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Nd1 | 0.0123 (3) | 0.0134 (3) | 0.0101 (3) | 0.0003 (3) | 0.0046 (2) | −0.0002 (3) |
O1 | 0.018 (4) | 0.026 (5) | 0.012 (4) | −0.003 (3) | 0.008 (3) | −0.002 (3) |
C1 | 0.020 (6) | 0.009 (5) | 0.011 (5) | 0.001 (4) | 0.008 (5) | 0.004 (4) |
O2 | 0.017 (4) | 0.023 (4) | 0.008 (3) | 0.008 (4) | 0.004 (3) | 0.002 (3) |
C2 | 0.021 (6) | 0.021 (6) | 0.014 (5) | 0.012 (5) | 0.013 (5) | 0.004 (5) |
O3 | 0.018 (4) | 0.017 (4) | 0.021 (4) | 0.007 (3) | 0.014 (3) | 0.008 (3) |
C3 | 0.013 (5) | 0.005 (5) | 0.014 (5) | 0.001 (4) | 0.008 (4) | −0.003 (4) |
O4 | 0.018 (4) | 0.016 (4) | 0.012 (4) | 0.005 (3) | 0.004 (3) | 0.004 (3) |
C4 | 0.007 (5) | 0.020 (6) | 0.022 (6) | −0.001 (4) | 0.006 (4) | 0.004 (5) |
O5 | 0.048 (6) | 0.024 (5) | 0.021 (4) | −0.006 (5) | 0.008 (4) | 0.005 (4) |
C5 | 0.009 (5) | 0.025 (7) | 0.024 (6) | 0.004 (5) | 0.000 (5) | 0.004 (5) |
O6 | 0.031 (5) | 0.014 (4) | 0.038 (5) | 0.000 (4) | 0.023 (4) | −0.005 (4) |
C6 | 0.009 (5) | 0.010 (5) | 0.013 (5) | 0.000 (5) | −0.002 (4) | 0.003 (4) |
O7 | 0.008 (4) | 0.016 (4) | 0.009 (3) | 0.004 (3) | −0.005 (3) | −0.001 (3) |
O8 | 0.036 (5) | 0.016 (4) | 0.014 (4) | −0.011 (4) | −0.003 (4) | 0.003 (3) |
Geometric parameters (Å, º) top
Nd1—O6i | 2.397 (8) | C2—H2B | 0.9700 |
Nd1—O8 | 2.427 (8) | O3—C6 | 1.271 (13) |
Nd1—O3 | 2.495 (7) | C3—O7 | 1.450 (12) |
Nd1—O2ii | 2.500 (7) | C3—C4 | 1.504 (14) |
Nd1—O4iii | 2.518 (7) | C3—C6 | 1.554 (14) |
Nd1—O1 | 2.540 (7) | O4—C6 | 1.236 (13) |
Nd1—O7 | 2.577 (8) | C4—C5 | 1.532 (16) |
Nd1—O1iv | 2.680 (7) | C4—H4A | 0.9700 |
Nd1—O2iv | 2.697 (7) | C4—H4B | 0.9700 |
O1—C1 | 1.243 (13) | O5—C5 | 1.245 (15) |
C1—O2 | 1.275 (12) | C5—O6 | 1.265 (14) |
C1—C2 | 1.510 (15) | O7—H7 | 0.8200 |
C2—C3 | 1.546 (14) | O8—H8A | 0.8501 |
C2—H2A | 0.9700 | O8—H8B | 0.8501 |
| | | |
O6i—Nd1—O8 | 144.5 (3) | O1—C1—O2 | 119.1 (10) |
O6i—Nd1—O3 | 69.1 (3) | O1—C1—C2 | 123.1 (9) |
O8—Nd1—O3 | 142.5 (3) | O2—C1—C2 | 117.8 (9) |
O6i—Nd1—O2ii | 75.3 (3) | C1—O2—Nd1v | 147.5 (7) |
O8—Nd1—O2ii | 110.0 (3) | C1—O2—Nd1iv | 95.5 (6) |
O3—Nd1—O2ii | 92.1 (2) | Nd1v—O2—Nd1iv | 114.7 (3) |
O6i—Nd1—O4iii | 139.1 (3) | C1—C2—C3 | 114.5 (8) |
O8—Nd1—O4iii | 69.8 (2) | C1—C2—H2A | 108.6 |
O3—Nd1—O4iii | 91.6 (3) | C3—C2—H2A | 108.6 |
O2ii—Nd1—O4iii | 69.6 (2) | C1—C2—H2B | 108.6 |
O6i—Nd1—O1 | 79.6 (3) | C3—C2—H2B | 108.6 |
O8—Nd1—O1 | 92.5 (3) | H2A—C2—H2B | 107.6 |
O3—Nd1—O1 | 75.5 (2) | C6—O3—Nd1 | 121.7 (6) |
O2ii—Nd1—O1 | 154.7 (3) | O7—C3—C4 | 110.9 (8) |
O4iii—Nd1—O1 | 131.6 (2) | O7—C3—C2 | 106.1 (8) |
O6i—Nd1—O7 | 124.2 (3) | C4—C3—C2 | 111.4 (9) |
O8—Nd1—O7 | 80.0 (3) | O7—C3—C6 | 109.5 (8) |
O3—Nd1—O7 | 62.8 (2) | C4—C3—C6 | 110.0 (8) |
O2ii—Nd1—O7 | 130.7 (2) | C2—C3—C6 | 108.9 (8) |
O4iii—Nd1—O7 | 69.6 (2) | C6—O4—Nd1i | 142.2 (7) |
O1—Nd1—O7 | 62.9 (2) | C3—C4—C5 | 112.8 (9) |
O6i—Nd1—O1iv | 77.7 (3) | C3—C4—H4A | 109.0 |
O8—Nd1—O1iv | 67.7 (3) | C5—C4—H4A | 109.0 |
O3—Nd1—O1iv | 132.1 (3) | C3—C4—H4B | 109.0 |
O2ii—Nd1—O1iv | 112.1 (2) | C5—C4—H4B | 109.0 |
O4iii—Nd1—O1iv | 134.9 (2) | H4A—C4—H4B | 107.8 |
O1—Nd1—O1iv | 65.1 (3) | O5—C5—O6 | 123.5 (12) |
O7—Nd1—O1iv | 116.0 (2) | O5—C5—C4 | 117.0 (11) |
O6i—Nd1—O2iv | 73.9 (3) | O6—C5—C4 | 119.5 (11) |
O8—Nd1—O2iv | 77.0 (3) | C5—O6—Nd1iii | 147.3 (8) |
O3—Nd1—O2iv | 140.5 (2) | O4—C6—O3 | 125.4 (10) |
O2ii—Nd1—O2iv | 65.3 (3) | O4—C6—C3 | 116.6 (9) |
O4iii—Nd1—O2iv | 108.2 (2) | O3—C6—C3 | 117.9 (9) |
O1—Nd1—O2iv | 111.0 (2) | C3—O7—Nd1 | 116.9 (6) |
O7—Nd1—O2iv | 155.9 (2) | C3—O7—H7 | 109.5 |
O1iv—Nd1—O2iv | 47.6 (2) | Nd1—O7—H7 | 110.5 |
C1—O1—Nd1 | 142.1 (7) | Nd1—O8—H8A | 109.3 |
C1—O1—Nd1iv | 97.2 (6) | Nd1—O8—H8B | 109.3 |
Nd1—O1—Nd1iv | 114.9 (3) | H8A—O8—H8B | 109.5 |
| | | |
O6i—Nd1—O1—C1 | −133.2 (12) | O2iv—Nd1—O3—C6 | 143.3 (7) |
O8—Nd1—O1—C1 | 81.6 (12) | C1—C2—C3—O7 | −47.4 (12) |
O3—Nd1—O1—C1 | −62.3 (11) | C1—C2—C3—C4 | −168.2 (9) |
O2ii—Nd1—O1—C1 | −125.1 (11) | C1—C2—C3—C6 | 70.4 (11) |
O4iii—Nd1—O1—C1 | 16.6 (13) | O7—C3—C4—C5 | 58.9 (11) |
O7—Nd1—O1—C1 | 4.2 (11) | C2—C3—C4—C5 | 176.9 (9) |
O1iv—Nd1—O1—C1 | 145.6 (13) | C6—C3—C4—C5 | −62.3 (11) |
O2iv—Nd1—O1—C1 | 158.6 (11) | C3—C4—C5—O5 | 53.7 (14) |
O6i—Nd1—O1—Nd1iv | 81.2 (3) | C3—C4—C5—O6 | −125.7 (11) |
O8—Nd1—O1—Nd1iv | −64.0 (3) | O5—C5—O6—Nd1iii | −81.6 (18) |
O3—Nd1—O1—Nd1iv | 152.1 (4) | C4—C5—O6—Nd1iii | 97.7 (17) |
O2ii—Nd1—O1—Nd1iv | 89.3 (6) | Nd1i—O4—C6—O3 | −25.5 (18) |
O4iii—Nd1—O1—Nd1iv | −128.9 (3) | Nd1i—O4—C6—C3 | 158.3 (8) |
O7—Nd1—O1—Nd1iv | −141.4 (4) | Nd1—O3—C6—O4 | −149.4 (8) |
O1iv—Nd1—O1—Nd1iv | 0.0 | Nd1—O3—C6—C3 | 26.8 (12) |
O2iv—Nd1—O1—Nd1iv | 13.1 (4) | O7—C3—C6—O4 | 176.9 (8) |
Nd1—O1—C1—O2 | −155.8 (8) | C4—C3—C6—O4 | −61.0 (12) |
Nd1iv—O1—C1—O2 | −7.0 (10) | C2—C3—C6—O4 | 61.3 (11) |
Nd1—O1—C1—C2 | 24.4 (18) | O7—C3—C6—O3 | 0.4 (12) |
Nd1iv—O1—C1—C2 | 173.2 (9) | C4—C3—C6—O3 | 122.5 (10) |
O1—C1—O2—Nd1v | 165.9 (8) | C2—C3—C6—O3 | −115.2 (10) |
C2—C1—O2—Nd1v | −14.2 (18) | C4—C3—O7—Nd1 | −146.8 (6) |
O1—C1—O2—Nd1iv | 6.9 (10) | C2—C3—O7—Nd1 | 92.1 (8) |
C2—C1—O2—Nd1iv | −173.3 (8) | C6—C3—O7—Nd1 | −25.2 (9) |
O1—C1—C2—C3 | −5.9 (15) | O6i—Nd1—O7—C3 | −6.1 (7) |
O2—C1—C2—C3 | 174.3 (9) | O8—Nd1—O7—C3 | −157.8 (6) |
O6i—Nd1—O3—C6 | 122.0 (8) | O3—Nd1—O7—C3 | 27.2 (6) |
O8—Nd1—O3—C6 | −37.1 (10) | O2ii—Nd1—O7—C3 | 94.3 (6) |
O2ii—Nd1—O3—C6 | −164.6 (8) | O4iii—Nd1—O7—C3 | 130.2 (6) |
O4iii—Nd1—O3—C6 | −95.0 (8) | O1—Nd1—O7—C3 | −59.8 (6) |
O1—Nd1—O3—C6 | 37.8 (8) | O1iv—Nd1—O7—C3 | −98.8 (6) |
O7—Nd1—O3—C6 | −28.9 (8) | O2iv—Nd1—O7—C3 | −140.6 (6) |
O1iv—Nd1—O3—C6 | 72.7 (9) | | |
Symmetry codes: (i) −x+1/2, y−1/2, −z+1/2; (ii) x, −y, z+1/2; (iii) −x+1/2, y+1/2, −z+1/2; (iv) −x, −y, −z; (v) x, −y, z−1/2. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O7—H7···O3iii | 0.82 | 1.89 | 2.668 (10) | 158 |
O8—H8B···O5iii | 0.85 | 1.88 | 2.665 (12) | 153 |
O8—H8A···O5vi | 0.85 | 1.97 | 2.653 (12) | 137 |
Symmetry codes: (iii) −x+1/2, y+1/2, −z+1/2; (vi) x−1/2, −y+1/2, z−1/2. |