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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

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536804032210/kp6015sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536804032210/kp6015Isup2.hkl
Contains datablock I

CCDC reference: 262257

Key indicators

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

Computing details top

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)]-µ5-citrato] top
Crystal data top
[Nd(C6H5O7)(H2O)]F(000) = 1336
Mr = 351.36Dx = 2.662 Mg m3
Monoclinic, C2/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2ycCell parameters from 1574 reflections
a = 16.6409 (11) Åθ = 2.7–25.0°
b = 8.7622 (6) ŵ = 5.95 mm1
c = 13.9279 (9) ÅT = 293 K
β = 120.288 (2)°Prism, colourless
V = 1753.6 (2) Å30.25 × 0.19 × 0.18 mm
Z = 8
Data collection top
Siemens SMART CCD area-detector
diffractometer
1507 independent reflections
Radiation source: fine-focus sealed tube1288 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.033
ω scansθmax = 25.0°, θmin = 2.7°
Absorption correction: empirical (using intensity measurements)
(SADABS; Sheldrick, 1996)
h = 1916
Tmin = 0.245, Tmax = 0.343k = 910
2359 measured reflectionsl = 1614
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)] = 0.046Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.109H-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 parametersΔρmax = 1.31 e Å3
0 restraintsΔρmin = 1.32 e Å3
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
xyzUiso*/Ueq
Nd10.08599 (4)0.08142 (7)0.17213 (4)0.0124 (2)
O10.0839 (5)0.0369 (9)0.0044 (6)0.0190 (17)
C10.1277 (8)0.0397 (12)0.0462 (8)0.013 (2)
O20.0849 (5)0.0752 (9)0.1490 (6)0.0171 (16)
C20.2302 (8)0.0034 (14)0.0084 (9)0.017 (2)
H2A0.23890.07390.03530.020*
H2B0.26290.09440.00740.020*
O30.2319 (5)0.0725 (9)0.2524 (6)0.0170 (16)
C30.2746 (7)0.0538 (11)0.1297 (8)0.011 (2)
O40.3276 (5)0.1922 (9)0.2091 (6)0.0167 (17)
C40.3703 (7)0.1181 (13)0.1703 (9)0.017 (2)
H4A0.36640.19790.11990.020*
H4B0.41010.03810.16930.020*
O50.4181 (7)0.0983 (10)0.3617 (7)0.035 (2)
C50.4143 (8)0.1838 (14)0.2881 (10)0.023 (3)
O60.4438 (6)0.3198 (9)0.3059 (7)0.0251 (19)
C60.2800 (7)0.0813 (13)0.2050 (8)0.014 (2)
O70.2125 (5)0.1700 (9)0.1295 (6)0.0152 (16)
H70.24310.23980.17120.018*
O80.0161 (6)0.3168 (9)0.0731 (6)0.029 (2)
H8A0.00450.30880.00650.035*
H8B0.05370.39020.10490.035*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Nd10.0123 (3)0.0134 (3)0.0101 (3)0.0003 (3)0.0046 (2)0.0002 (3)
O10.018 (4)0.026 (5)0.012 (4)0.003 (3)0.008 (3)0.002 (3)
C10.020 (6)0.009 (5)0.011 (5)0.001 (4)0.008 (5)0.004 (4)
O20.017 (4)0.023 (4)0.008 (3)0.008 (4)0.004 (3)0.002 (3)
C20.021 (6)0.021 (6)0.014 (5)0.012 (5)0.013 (5)0.004 (5)
O30.018 (4)0.017 (4)0.021 (4)0.007 (3)0.014 (3)0.008 (3)
C30.013 (5)0.005 (5)0.014 (5)0.001 (4)0.008 (4)0.003 (4)
O40.018 (4)0.016 (4)0.012 (4)0.005 (3)0.004 (3)0.004 (3)
C40.007 (5)0.020 (6)0.022 (6)0.001 (4)0.006 (4)0.004 (5)
O50.048 (6)0.024 (5)0.021 (4)0.006 (5)0.008 (4)0.005 (4)
C50.009 (5)0.025 (7)0.024 (6)0.004 (5)0.000 (5)0.004 (5)
O60.031 (5)0.014 (4)0.038 (5)0.000 (4)0.023 (4)0.005 (4)
C60.009 (5)0.010 (5)0.013 (5)0.000 (5)0.002 (4)0.003 (4)
O70.008 (4)0.016 (4)0.009 (3)0.004 (3)0.005 (3)0.001 (3)
O80.036 (5)0.016 (4)0.014 (4)0.011 (4)0.003 (4)0.003 (3)
Geometric parameters (Å, º) top
Nd1—O6i2.397 (8)C2—H2B0.9700
Nd1—O82.427 (8)O3—C61.271 (13)
Nd1—O32.495 (7)C3—O71.450 (12)
Nd1—O2ii2.500 (7)C3—C41.504 (14)
Nd1—O4iii2.518 (7)C3—C61.554 (14)
Nd1—O12.540 (7)O4—C61.236 (13)
Nd1—O72.577 (8)C4—C51.532 (16)
Nd1—O1iv2.680 (7)C4—H4A0.9700
Nd1—O2iv2.697 (7)C4—H4B0.9700
O1—C11.243 (13)O5—C51.245 (15)
C1—O21.275 (12)C5—O61.265 (14)
C1—C21.510 (15)O7—H70.8200
C2—C31.546 (14)O8—H8A0.8501
C2—H2A0.9700O8—H8B0.8501
O6i—Nd1—O8144.5 (3)O1—C1—O2119.1 (10)
O6i—Nd1—O369.1 (3)O1—C1—C2123.1 (9)
O8—Nd1—O3142.5 (3)O2—C1—C2117.8 (9)
O6i—Nd1—O2ii75.3 (3)C1—O2—Nd1v147.5 (7)
O8—Nd1—O2ii110.0 (3)C1—O2—Nd1iv95.5 (6)
O3—Nd1—O2ii92.1 (2)Nd1v—O2—Nd1iv114.7 (3)
O6i—Nd1—O4iii139.1 (3)C1—C2—C3114.5 (8)
O8—Nd1—O4iii69.8 (2)C1—C2—H2A108.6
O3—Nd1—O4iii91.6 (3)C3—C2—H2A108.6
O2ii—Nd1—O4iii69.6 (2)C1—C2—H2B108.6
O6i—Nd1—O179.6 (3)C3—C2—H2B108.6
O8—Nd1—O192.5 (3)H2A—C2—H2B107.6
O3—Nd1—O175.5 (2)C6—O3—Nd1121.7 (6)
O2ii—Nd1—O1154.7 (3)O7—C3—C4110.9 (8)
O4iii—Nd1—O1131.6 (2)O7—C3—C2106.1 (8)
O6i—Nd1—O7124.2 (3)C4—C3—C2111.4 (9)
O8—Nd1—O780.0 (3)O7—C3—C6109.5 (8)
O3—Nd1—O762.8 (2)C4—C3—C6110.0 (8)
O2ii—Nd1—O7130.7 (2)C2—C3—C6108.9 (8)
O4iii—Nd1—O769.6 (2)C6—O4—Nd1i142.2 (7)
O1—Nd1—O762.9 (2)C3—C4—C5112.8 (9)
O6i—Nd1—O1iv77.7 (3)C3—C4—H4A109.0
O8—Nd1—O1iv67.7 (3)C5—C4—H4A109.0
O3—Nd1—O1iv132.1 (3)C3—C4—H4B109.0
O2ii—Nd1—O1iv112.1 (2)C5—C4—H4B109.0
O4iii—Nd1—O1iv134.9 (2)H4A—C4—H4B107.8
O1—Nd1—O1iv65.1 (3)O5—C5—O6123.5 (12)
O7—Nd1—O1iv116.0 (2)O5—C5—C4117.0 (11)
O6i—Nd1—O2iv73.9 (3)O6—C5—C4119.5 (11)
O8—Nd1—O2iv77.0 (3)C5—O6—Nd1iii147.3 (8)
O3—Nd1—O2iv140.5 (2)O4—C6—O3125.4 (10)
O2ii—Nd1—O2iv65.3 (3)O4—C6—C3116.6 (9)
O4iii—Nd1—O2iv108.2 (2)O3—C6—C3117.9 (9)
O1—Nd1—O2iv111.0 (2)C3—O7—Nd1116.9 (6)
O7—Nd1—O2iv155.9 (2)C3—O7—H7109.5
O1iv—Nd1—O2iv47.6 (2)Nd1—O7—H7110.5
C1—O1—Nd1142.1 (7)Nd1—O8—H8A109.3
C1—O1—Nd1iv97.2 (6)Nd1—O8—H8B109.3
Nd1—O1—Nd1iv114.9 (3)H8A—O8—H8B109.5
O6i—Nd1—O1—C1133.2 (12)O2iv—Nd1—O3—C6143.3 (7)
O8—Nd1—O1—C181.6 (12)C1—C2—C3—O747.4 (12)
O3—Nd1—O1—C162.3 (11)C1—C2—C3—C4168.2 (9)
O2ii—Nd1—O1—C1125.1 (11)C1—C2—C3—C670.4 (11)
O4iii—Nd1—O1—C116.6 (13)O7—C3—C4—C558.9 (11)
O7—Nd1—O1—C14.2 (11)C2—C3—C4—C5176.9 (9)
O1iv—Nd1—O1—C1145.6 (13)C6—C3—C4—C562.3 (11)
O2iv—Nd1—O1—C1158.6 (11)C3—C4—C5—O553.7 (14)
O6i—Nd1—O1—Nd1iv81.2 (3)C3—C4—C5—O6125.7 (11)
O8—Nd1—O1—Nd1iv64.0 (3)O5—C5—O6—Nd1iii81.6 (18)
O3—Nd1—O1—Nd1iv152.1 (4)C4—C5—O6—Nd1iii97.7 (17)
O2ii—Nd1—O1—Nd1iv89.3 (6)Nd1i—O4—C6—O325.5 (18)
O4iii—Nd1—O1—Nd1iv128.9 (3)Nd1i—O4—C6—C3158.3 (8)
O7—Nd1—O1—Nd1iv141.4 (4)Nd1—O3—C6—O4149.4 (8)
O1iv—Nd1—O1—Nd1iv0.0Nd1—O3—C6—C326.8 (12)
O2iv—Nd1—O1—Nd1iv13.1 (4)O7—C3—C6—O4176.9 (8)
Nd1—O1—C1—O2155.8 (8)C4—C3—C6—O461.0 (12)
Nd1iv—O1—C1—O27.0 (10)C2—C3—C6—O461.3 (11)
Nd1—O1—C1—C224.4 (18)O7—C3—C6—O30.4 (12)
Nd1iv—O1—C1—C2173.2 (9)C4—C3—C6—O3122.5 (10)
O1—C1—O2—Nd1v165.9 (8)C2—C3—C6—O3115.2 (10)
C2—C1—O2—Nd1v14.2 (18)C4—C3—O7—Nd1146.8 (6)
O1—C1—O2—Nd1iv6.9 (10)C2—C3—O7—Nd192.1 (8)
C2—C1—O2—Nd1iv173.3 (8)C6—C3—O7—Nd125.2 (9)
O1—C1—C2—C35.9 (15)O6i—Nd1—O7—C36.1 (7)
O2—C1—C2—C3174.3 (9)O8—Nd1—O7—C3157.8 (6)
O6i—Nd1—O3—C6122.0 (8)O3—Nd1—O7—C327.2 (6)
O8—Nd1—O3—C637.1 (10)O2ii—Nd1—O7—C394.3 (6)
O2ii—Nd1—O3—C6164.6 (8)O4iii—Nd1—O7—C3130.2 (6)
O4iii—Nd1—O3—C695.0 (8)O1—Nd1—O7—C359.8 (6)
O1—Nd1—O3—C637.8 (8)O1iv—Nd1—O7—C398.8 (6)
O7—Nd1—O3—C628.9 (8)O2iv—Nd1—O7—C3140.6 (6)
O1iv—Nd1—O3—C672.7 (9)
Symmetry codes: (i) x+1/2, y1/2, 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, z1/2.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O7—H7···O3iii0.821.892.668 (10)158
O8—H8B···O5iii0.851.882.665 (12)153
O8—H8A···O5vi0.851.972.653 (12)137
Symmetry codes: (iii) x+1/2, y+1/2, z+1/2; (vi) x1/2, y+1/2, z1/2.
 

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