Key indicators
- Single-crystal X-ray study
- T = 150 K
- Mean (C-C) = 0.009 Å
Some non-H atoms missing
- Disorder in main residue
- R factor = 0.043
- wR factor = 0.122
- Data-to-parameter ratio = 22.5
checkCIF/PLATON results
No syntax errors found
Alert level A
PLAT220_ALERT_2_A Large Non-Solvent C Ueq(max)/Ueq(min) ... 5.50 Ratio
| Author Response: Atom belongs to disordered ligand which been modelled over
two sites
|
PLAT221_ALERT_4_A Large Solvent/Anion O Ueq(max)/Ueq(min) ... 5.27 Ratio
| Author Response: Atom belongs to disordered ligand which been modelled over
two sites
|
PLAT222_ALERT_3_A Large Non-Solvent H Ueq(max)/Ueq(min) ... 7.82 Ratio
| Author Response: Atom belongs to disordered ligand which been modelled over
two sites
|
Alert level B
CHEMW03_ALERT_2_B WARNING: The ratio of given/expected molecular weight as
calculated from the _atom_site* data lies outside
the range 0.95 <> 1.05
From the CIF: _cell_formula_units_Z 4
From the CIF: _chemical_formula_weight 1931.64
TEST: Calculate formula weight from _atom_site_*
atom mass num sum
C 12.01 36.00 432.40
H 1.01 48.00 48.38
O 16.00 40.00 639.96
Cl 35.45 4.00 141.81
Nd 144.24 4.00 576.96
Calculated formula weight 1839.51
PLAT043_ALERT_1_B Check Reported Molecular Weight ................ 1931.64
| Author Response: Reported Molecular Weight includes two molecules of ethanol
which were removed using the SQUEEZE option in PLATON (Spek, 2003)
|
PLAT201_ALERT_2_B Isotropic non-H Atoms in Main Residue(s) ....... 1
| Author Response: Disordered atom modelled with isotropic diplacement
parameters
|
PLAT241_ALERT_2_B Check High Ueq as Compared to Neighbors for C10
| Author Response: Atom belongs to disordered ligand which been modelled over
two sites
|
PLAT420_ALERT_2_B D-H Without Acceptor O11 - H11B ... ?
| Author Response: The acceptor O atom could be from the hydroxy group od
the disordered ethanol which has been removed.
|
Alert level C
PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings Differ .... ?
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ?
PLAT044_ALERT_1_C Calculated and Reported Dx Differ .............. ?
PLAT068_ALERT_1_C Reported F000 Differs from Calcd (or Missing)... ?
PLAT152_ALERT_1_C Supplied and Calc Volume s.u. Inconsistent ..... ?
PLAT165_ALERT_3_C Nr. of Status R Flagged Non-Hydrogen Atoms ..... 1
PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C11
PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C14
PLAT243_ALERT_4_C High 'Solvent' Ueq as Compared to Neighbors for O18
PLAT250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor .... 2.10
PLAT301_ALERT_3_C Main Residue Disorder ......................... 15.00 Perc.
PLAT302_ALERT_4_C Anion/Solvent Disorder ......................... 29.00 Perc.
PLAT342_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 9
PLAT602_ALERT_4_C VERY LARGE Solvent Accessible VOID(S) in Structure !
| Author Response: The removed disordered ethanol molecules reside
in these voids.
|
PLAT751_ALERT_4_C Bond Calc 2.62746, Rep 2.627(3) ...... Senseless su
ND2 -O12 1.555 1.555
PLAT752_ALERT_4_C Angle Calc 146.22, Rep 146.21(10) ...... Senseless su
O8 -ND2 -O12 1.555 1.555 1.555
PLAT752_ALERT_4_C Angle Calc 69.44, Rep 69.45(11) ...... Senseless su
O6 -ND2 -O12 1.555 1.555 1.555
PLAT752_ALERT_4_C Angle Calc 75.18, Rep 75.19(10) ...... Senseless su
O9 -ND2 -O12 1.555 1.555 1.555
PLAT752_ALERT_4_C Angle Calc 67.91, Rep 67.92(11) ...... Senseless su
O1 -ND2 -O12 1.555 1.555 1.555
PLAT752_ALERT_4_C Angle Calc 131.69, Rep 131.68(12) ...... Senseless su
O13 -ND2 -O12 1.555 1.555 1.555
PLAT752_ALERT_4_C Angle Calc 118.72, Rep 118.72(6) ...... Senseless su
O7 -ND2 -O12 1.555 1.555 1.555
PLAT752_ALERT_4_C Angle Calc 115.51, Rep 115.50(10) ...... Senseless su
O2 -ND2 -O12 1.555 1.555 1.555
PLAT752_ALERT_4_C Angle Calc 114.73, Rep 114.73(7) ...... Senseless su
O12 -ND2 -ND1 1.555 1.555 1.555
PLAT757_ALERT_4_C D...A Calc 2.76446, Rep 2.764(5) ...... Senseless su
O10 -O12 1.555 2.555
PLAT757_ALERT_4_C D...A Calc 2.81912, Rep 2.819(6) ...... Senseless su
O12 -O16 1.555 2.555
PLAT764_ALERT_4_C Overcomplete CIF Bond List Detected (Rep/Expd) . 1.14 Ratio
PLAT779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ...... 5.10 Deg.
C12 -O5 -C12 1.555 1.555 2.555
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: C40 H60 Cl4 Nd4 O42
Atom count from _chemical_formula_moiety:C42 H66 Cl8 Nd4 O58
FORMU01_ALERT_2_G There is a discrepancy between the atom counts in the
_chemical_formula_sum and the formula from the _atom_site* data.
Atom count from _chemical_formula_sum:C40 H60 Cl4 Nd4 O42
Atom count from the _atom_site data: C36 H48 Cl4 Nd4 O40
CELLZ01_ALERT_1_G Difference between formula and atom_site contents detected.
CELLZ01_ALERT_1_G ALERT: Large difference may be due to a
symmetry error - see SYMMG tests
From the CIF: _cell_formula_units_Z 4
From the CIF: _chemical_formula_sum C40 H60 Cl4 Nd4 O42
TEST: Compare cell contents of formula and atom_site data
atom Z*formula cif sites diff
C 160.00 144.00 16.00
H 240.00 192.00 48.00
Cl 16.00 16.00 0.00
Nd 16.00 16.00 0.00
O 168.00 160.00 8.00
3 ALERT level A = In general: serious problem
5 ALERT level B = Potentially serious problem
27 ALERT level C = Check and explain
4 ALERT level G = General alerts; check
9 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
10 ALERT type 2 Indicator that the structure model may be wrong or deficient
4 ALERT type 3 Indicator that the structure quality may be low
16 ALERT type 4 Improvement, methodology, query or suggestion
NaOH (2 mmol, 0.08 g) in methanol (10 ml) was added in five portions to a boiling solution of Nd(ClO4)3.nH2O (8 mmol, 1.346 g N d2O3) in methanol (10 ml). A solution of 2,6-diformyl-4-methylphenol (4 mmol, 0.6566 g) and NaOH (4 mmol, 0.16 g) in methanol (150 ml) was then added to the boiling solution in 20 ml portions. After each addition of sodium cresolate, the mixture was boiled until approximately 10 ml of solution remained before adding the next 20 ml portion. The pH of the mixture at this point was approximately 6.5. The final mixture was boiled until 5 ml of solution remained. It was then cooled and filtered and approximately 10 ml of ethanol was added. The resulting mixture was left in an open flask at room temperature. The onset of crystallization was obvious after 3 d but a further 2 d were allowed for the process to proceed to completion. Yellow blocks of (I) were recovered in 20% yield (calculation based on LnIII). The crystals lost solvent and crumbled to an amorphous solid on exposure to air. CAUTION: Although no problems were encountered in this work, perchlorate compounds are potentially explosive. They should be prepared in small amounts and handled with care.
One of the percholate anions (Cl2/O18/O19/O20/O21) is disordered over two sites, with an occupancy ratio of 0.577 (4)/0.423 (4) for the major and minor components. Both components of disorder have the site of O18 in common. In addition, one of the µ2-C9H7O3 ligands (containing the benzene ring C11/C11A/C12/C13/C13A/C14) is also disordered; initial refinement gave equal values within experimental error for the two disorder components; the occupancy ratio was therefore fixed at 0.5:0.5 in the final cycles. This disordered ligand is bisected by the crystallographic twofold axis but the disorder is not imposed by the crystallographic symmetry. All H atoms bonded to C atoms were placed in calculated positions, with C—H distances of 0.95 or 0.98 Å (methyl), and were included in the refinement in the riding-model approximation, with Uiso(H) = 1.2Ueq(C), or 1.5Ueq(C) for methyl H atoms. The H atoms of the bridging hydroxyl ligands were included with O—H = 1.00 Å and Uiso(H) = 1.2Ueq(O). All other H atoms bonded to O atoms were placed in calculated positions based on an ideal location for O—H···O hydrogen bonding. The O—H distance was fixed at 0.84 Å with Uiso(H) = 1.5Ueq(O). During the refinement, areas of electron density were located in difference Fourier maps that were assigned as ethanol solvent molecules. The peak pattern of electron density suggested that the solvent molecules were highly disordered, and attempts to model the disorder were unsuccessful. In the final cycles of refinement, the contribution to electron density corresesponding to the disordered ethanol molecules was removed from the observed data using the SQUEEZE option in PLATON (Spek, 2003). The resulting data vastly improved the precision of the geometric parameters of the remaining structure. The contributions of two molecules of ethanol have been included in the molecular formula. The hydroxy groups of the ethanol molecules, if present, would contribute to the hydrogen-bonding motif, and for that reason the hydrogen bonding in the title structure is not discussed in detail. In the final difference Fourier map, the three largest density peaks in the range 1.64–1.06 e Å3 were located within 1.23 Å of the disordered perchlorate anion, and the deepest hole of −1.16 e Å3 was 0.80 Å from Nd1.
Data collection: COLLECT (Nonius, 2002); cell refinement: DENZO-SMN (Otwinowski & Minor, 1997); data reduction: DENZO-SMN; program(s) used to solve structure: SHELXTL/PC (Sheldrick, 2001); program(s) used to refine structure: SHELXTL/PC; molecular graphics: SHELXTL/PC; software used to prepare material for publication: SHELXTL/PC.
Tetrakis(µ
2-2,6-diformyl-4-methylphenolato)tetra-µ
3-hydroxo- tetrakis[diaquaneodymium(III)] tetrakis(perchlorate) ethanol disolvate
top
Crystal data top
[Nd4(C9H7O3)4(OH)4(H2O)8](ClO4)4·2C2H6O | F(000) = 3776 |
Mr = 1931.64 | Dx = 1.620 Mg m−3 |
Monoclinic, C2/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -C 2yc | Cell parameters from 8715 reflections |
a = 20.9933 (3) Å | θ = 2.6–27.5° |
b = 24.7385 (5) Å | µ = 2.80 mm−1 |
c = 17.6893 (3) Å | T = 150 K |
β = 120.469 (1)° | Block, yellow |
V = 7918.1 (2) Å3 | 0.32 × 0.28 × 0.25 mm |
Z = 4 | |
Data collection top
Bruker Nonius KappaCCD area detector diffractometer | 8998 independent reflections |
Radiation source: fine-focus sealed tube | 7708 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.037 |
Detector resolution: 9 pixels mm-1 | θmax = 27.5°, θmin = 2.6° |
ϕ scans and ω scans with κ offsets | h = −27→27 |
Absorption correction: multi-scan (DENZO-SMN; Otwinowski & Minor, 1997) | k = −32→32 |
Tmin = 0.430, Tmax = 0.497 | l = −22→19 |
31251 measured reflections | |
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)] = 0.043 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.122 | H-atom parameters constrained |
S = 1.06 | w = 1/[σ2(Fo2) + (0.0625P)2 + 41.2001P] where P = (Fo2 + 2Fc2)/3 |
8998 reflections | (Δ/σ)max < 0.001 |
400 parameters | Δρmax = 1.64 e Å−3 |
55 restraints | Δρmin = −1.16 e Å−3 |
Crystal data top
[Nd4(C9H7O3)4(OH)4(H2O)8](ClO4)4·2C2H6O | V = 7918.1 (2) Å3 |
Mr = 1931.64 | Z = 4 |
Monoclinic, C2/c | Mo Kα radiation |
a = 20.9933 (3) Å | µ = 2.80 mm−1 |
b = 24.7385 (5) Å | T = 150 K |
c = 17.6893 (3) Å | 0.32 × 0.28 × 0.25 mm |
β = 120.469 (1)° | |
Data collection top
Bruker Nonius KappaCCD area detector diffractometer | 8998 independent reflections |
Absorption correction: multi-scan (DENZO-SMN; Otwinowski & Minor, 1997) | 7708 reflections with I > 2σ(I) |
Tmin = 0.430, Tmax = 0.497 | Rint = 0.037 |
31251 measured reflections | |
Refinement top
R[F2 > 2σ(F2)] = 0.043 | 55 restraints |
wR(F2) = 0.122 | H-atom parameters constrained |
S = 1.06 | w = 1/[σ2(Fo2) + (0.0625P)2 + 41.2001P] where P = (Fo2 + 2Fc2)/3 |
8998 reflections | Δρmax = 1.64 e Å−3 |
400 parameters | Δρmin = −1.16 e Å−3 |
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 | x | y | z | Uiso*/Ueq | Occ. (<1) |
Nd1 | −0.103278 (13) | 0.226744 (11) | 0.186982 (16) | 0.02998 (10) | |
Nd2 | −0.027319 (12) | 0.108328 (10) | 0.334350 (15) | 0.02776 (10) | |
O1 | −0.0765 (2) | 0.11184 (16) | 0.4338 (2) | 0.0395 (8) | |
O2 | −0.14590 (17) | 0.16722 (15) | 0.2703 (2) | 0.0344 (7) | |
O3 | −0.2398 (2) | 0.23177 (18) | 0.1173 (2) | 0.0439 (9) | |
O4 | −0.1409 (7) | 0.3076 (5) | 0.0936 (8) | 0.052 (3)* | 0.50 |
O4A | 0.1476 (7) | 0.3110 (4) | 0.3937 (8) | 0.052 (3)* | 0.50 |
O5 | 0.0000 | 0.2977 (2) | 0.2500 | 0.0396 (11)* | |
O6 | 0.0205 (2) | 0.02579 (15) | 0.4208 (2) | 0.0391 (8) | |
O7 | 0.0000 | 0.03688 (18) | 0.2500 | 0.0324 (10) | |
O8 | −0.07912 (17) | 0.12937 (14) | 0.1823 (2) | 0.0284 (6) | |
H8 | −0.1244 | 0.1079 | 0.1426 | 0.034* | |
O9 | −0.00252 (16) | 0.20477 (14) | 0.3318 (2) | 0.0285 (7) | |
H9 | −0.0032 | 0.2259 | 0.3796 | 0.034* | |
O10 | −0.1661 (2) | 0.20022 (19) | 0.0304 (2) | 0.0482 (10) | |
H10C | −0.1925 | 0.2232 | −0.0078 | 0.072* | |
H10D | −0.1512 | 0.1759 | 0.0098 | 0.072* | |
O11 | −0.13126 (15) | 0.28884 (12) | 0.27878 (18) | 0.0536 (10) | |
H11A | −0.1219 | 0.2757 | 0.3271 | 0.080* | |
H11B | −0.1052 | 0.3137 | 0.2761 | 0.080* | |
O12 | 0.07556 (15) | 0.13128 (12) | 0.49605 (18) | 0.0387 (8) | |
H12A | 0.0967 | 0.1057 | 0.5312 | 0.058* | |
H12B | 0.0611 | 0.1550 | 0.5180 | 0.058* | |
O13 | −0.1336 (2) | 0.04277 (17) | 0.2737 (3) | 0.0479 (9) | |
H13C | −0.1477 | 0.0260 | 0.2265 | 0.072* | |
H13D | −0.1381 | 0.0188 | 0.3043 | 0.072* | |
C1 | −0.2034 (2) | 0.1666 (2) | 0.2790 (3) | 0.0326 (10) | |
C2 | −0.2017 (3) | 0.1420 (2) | 0.3531 (3) | 0.0347 (10) | |
C3 | −0.2658 (3) | 0.1411 (2) | 0.3600 (4) | 0.0437 (13) | |
H3A | −0.2628 | 0.1250 | 0.4105 | 0.052* | |
C4 | −0.3324 (3) | 0.1625 (3) | 0.2971 (5) | 0.0513 (15) | |
C5 | −0.3348 (3) | 0.1861 (3) | 0.2255 (4) | 0.0534 (16) | |
H5A | −0.3804 | 0.2007 | 0.1811 | 0.064* | |
C6 | −0.2728 (3) | 0.1895 (3) | 0.2149 (4) | 0.0420 (12) | |
C7 | −0.1373 (3) | 0.1197 (2) | 0.4260 (3) | 0.0386 (11) | |
H7A | −0.1420 | 0.1096 | 0.4748 | 0.046* | |
C8 | −0.3995 (4) | 0.1604 (4) | 0.3076 (6) | 0.073 (2) | |
H8A | −0.4444 | 0.1618 | 0.2497 | 0.109* | |
H8B | −0.3987 | 0.1914 | 0.3426 | 0.109* | |
H8C | −0.3988 | 0.1268 | 0.3374 | 0.109* | |
C9 | −0.2853 (3) | 0.2185 (3) | 0.1380 (4) | 0.0512 (15) | |
H9A | −0.3350 | 0.2287 | 0.0983 | 0.061* | |
C10 | −0.1264 (8) | 0.3536 (7) | 0.1237 (8) | 0.103 (11)* | 0.50 |
H10A | −0.1662 | 0.3777 | 0.0904 | 0.123* | 0.50 |
C11 | −0.0651 (4) | 0.3807 (4) | 0.1961 (5) | 0.057 (3)* | 0.50 |
C12 | −0.0002 (5) | 0.3493 (3) | 0.2531 (6) | 0.060 (2)* | 0.50 |
C13 | −0.0683 (8) | 0.4366 (5) | 0.2112 (8) | 0.073 (4)* | 0.50 |
H13A | −0.1120 | 0.4558 | 0.1722 | 0.087* | 0.50 |
C10A | 0.1278 (6) | 0.3582 (5) | 0.3887 (8) | 0.052 (4)* | 0.50 |
H10B | 0.1619 | 0.3824 | 0.4321 | 0.063* | 0.50 |
C11A | 0.0578 (6) | 0.3803 (5) | 0.3235 (7) | 0.066 (4)* | 0.50 |
C13A | 0.0519 (8) | 0.4362 (5) | 0.3357 (9) | 0.078 (4)* | 0.50 |
H13B | 0.0921 | 0.4544 | 0.3833 | 0.094* | 0.50 |
C14 | −0.0113 (6) | 0.4648 (6) | 0.2795 (7) | 0.085 (5)* | 0.50 |
C15 | −0.0180 (10) | 0.5246 (7) | 0.2923 (11) | 0.177 (14)* | 0.50 |
H15A | 0.0175 | 0.5447 | 0.2826 | 0.266* | 0.50 |
H15B | −0.0075 | 0.5311 | 0.3522 | 0.266* | 0.50 |
H15C | −0.0682 | 0.5368 | 0.2504 | 0.266* | 0.50 |
C16 | 0.0191 (3) | −0.0224 (2) | 0.4036 (3) | 0.0389 (11) | |
H16A | 0.0264 | −0.0470 | 0.4485 | 0.047* | |
C17 | 0.0000 | −0.0147 (2) | 0.2500 | 0.0324 (14) | |
C18 | 0.0074 (3) | −0.0459 (2) | 0.3228 (3) | 0.0378 (11) | |
C19 | 0.0070 (4) | −0.1030 (2) | 0.3205 (4) | 0.0516 (15) | |
H19A | 0.0118 | −0.1222 | 0.3696 | 0.062* | |
C20 | 0.0000 | −0.1322 (4) | 0.2500 | 0.061 (2) | |
C21 | 0.0000 | −0.1934 (4) | 0.2500 | 0.085 (4) | |
H21A | −0.0242 | −0.2066 | 0.1894 | 0.127* | 0.50 |
H21B | −0.0268 | −0.2066 | 0.2783 | 0.127* | 0.50 |
H21C | 0.0510 | −0.2066 | 0.2823 | 0.127* | 0.50 |
Cl1 | 0.02244 (8) | 0.25412 (7) | −0.02193 (10) | 0.0527 (4) | |
O14 | 0.0939 (4) | 0.2368 (3) | 0.0294 (8) | 0.155 (5) | |
O15 | −0.0054 (6) | 0.2765 (3) | 0.0325 (5) | 0.115 (3) | |
O16 | −0.0269 (3) | 0.2106 (2) | −0.0698 (3) | 0.0719 (15) | |
O17 | 0.0176 (3) | 0.2957 (2) | −0.0789 (3) | 0.0623 (12) | |
Cl2 | 0.22322 (13) | 0.01002 (11) | 0.47137 (18) | 0.0525 (8) | 0.577 (4) |
O18 | 0.2017 (5) | −0.0118 (3) | 0.5303 (5) | 0.120 (3) | |
O19 | 0.2059 (5) | 0.0655 (4) | 0.4521 (11) | 0.141 (7) | 0.577 (4) |
O20 | 0.1816 (6) | −0.0144 (5) | 0.3858 (6) | 0.093 (3) | 0.577 (4) |
O21 | 0.2993 (4) | −0.0008 (6) | 0.5071 (8) | 0.102 (4) | 0.577 (4) |
Cl2A | 0.2145 (3) | 0.0225 (2) | 0.6070 (3) | 0.0799 (16) | 0.423 (4) |
O19A | 0.1495 (4) | 0.0416 (4) | 0.6196 (5) | 0.037 (2) | 0.423 (4) |
O20A | 0.2328 (15) | 0.0773 (7) | 0.5976 (19) | 0.152 (9)* | 0.423 (4) |
O21A | 0.2763 (14) | 0.0035 (13) | 0.6900 (14) | 0.195 (12)* | 0.423 (4) |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Nd1 | 0.02135 (14) | 0.04034 (17) | 0.02491 (15) | 0.00338 (9) | 0.00928 (11) | 0.00406 (10) |
Nd2 | 0.02325 (14) | 0.03795 (16) | 0.02207 (14) | 0.00186 (9) | 0.01149 (11) | 0.00229 (9) |
O1 | 0.0303 (17) | 0.058 (2) | 0.0329 (19) | 0.0096 (16) | 0.0180 (16) | 0.0085 (16) |
O2 | 0.0217 (15) | 0.051 (2) | 0.0314 (17) | 0.0047 (14) | 0.0140 (14) | 0.0071 (15) |
O3 | 0.0270 (17) | 0.070 (3) | 0.0312 (19) | 0.0066 (16) | 0.0121 (15) | 0.0104 (18) |
O6 | 0.046 (2) | 0.041 (2) | 0.0283 (18) | 0.0045 (16) | 0.0171 (16) | 0.0026 (15) |
O7 | 0.032 (2) | 0.036 (2) | 0.029 (2) | 0.000 | 0.016 (2) | 0.000 |
O8 | 0.0220 (14) | 0.0371 (17) | 0.0242 (15) | −0.0003 (13) | 0.0104 (13) | 0.0022 (13) |
O9 | 0.0216 (14) | 0.0388 (17) | 0.0240 (15) | −0.0007 (12) | 0.0108 (13) | −0.0050 (13) |
O10 | 0.041 (2) | 0.069 (3) | 0.0272 (18) | 0.0221 (19) | 0.0117 (16) | 0.0093 (18) |
O11 | 0.045 (2) | 0.066 (3) | 0.048 (2) | 0.007 (2) | 0.022 (2) | −0.006 (2) |
O12 | 0.0358 (18) | 0.051 (2) | 0.0270 (17) | 0.0054 (16) | 0.0139 (15) | 0.0021 (16) |
O13 | 0.042 (2) | 0.055 (2) | 0.048 (2) | −0.0087 (18) | 0.0232 (19) | −0.0044 (19) |
C1 | 0.022 (2) | 0.046 (3) | 0.027 (2) | 0.0007 (19) | 0.0113 (18) | 0.000 (2) |
C2 | 0.028 (2) | 0.045 (3) | 0.035 (3) | 0.003 (2) | 0.019 (2) | 0.001 (2) |
C3 | 0.037 (3) | 0.056 (3) | 0.052 (3) | 0.001 (2) | 0.032 (3) | 0.007 (3) |
C4 | 0.034 (3) | 0.063 (4) | 0.067 (4) | 0.003 (3) | 0.033 (3) | 0.010 (3) |
C5 | 0.028 (3) | 0.076 (4) | 0.056 (4) | 0.008 (3) | 0.022 (3) | 0.016 (3) |
C6 | 0.023 (2) | 0.061 (3) | 0.041 (3) | 0.005 (2) | 0.015 (2) | 0.010 (3) |
C7 | 0.038 (3) | 0.052 (3) | 0.032 (3) | 0.004 (2) | 0.022 (2) | 0.008 (2) |
C8 | 0.042 (3) | 0.099 (6) | 0.097 (6) | 0.016 (3) | 0.050 (4) | 0.037 (5) |
C9 | 0.025 (2) | 0.081 (4) | 0.041 (3) | 0.009 (3) | 0.011 (2) | 0.014 (3) |
C16 | 0.040 (3) | 0.044 (3) | 0.030 (2) | 0.006 (2) | 0.016 (2) | 0.008 (2) |
C17 | 0.028 (3) | 0.036 (3) | 0.031 (3) | 0.000 | 0.013 (3) | 0.000 |
C18 | 0.043 (3) | 0.036 (3) | 0.033 (3) | 0.004 (2) | 0.018 (2) | 0.004 (2) |
C19 | 0.071 (4) | 0.040 (3) | 0.051 (4) | 0.001 (3) | 0.037 (3) | 0.006 (3) |
C20 | 0.093 (8) | 0.041 (5) | 0.064 (6) | 0.000 | 0.051 (6) | 0.000 |
C21 | 0.152 (13) | 0.045 (5) | 0.079 (8) | 0.000 | 0.074 (9) | 0.000 |
Cl1 | 0.0417 (7) | 0.0663 (9) | 0.0414 (7) | −0.0043 (6) | 0.0147 (6) | 0.0137 (7) |
O14 | 0.046 (3) | 0.110 (6) | 0.230 (11) | 0.009 (3) | 0.012 (5) | 0.083 (7) |
O15 | 0.219 (9) | 0.081 (4) | 0.105 (5) | 0.006 (5) | 0.126 (7) | 0.008 (4) |
O16 | 0.091 (4) | 0.074 (3) | 0.054 (3) | −0.029 (3) | 0.039 (3) | −0.002 (3) |
O17 | 0.058 (3) | 0.080 (3) | 0.054 (3) | −0.011 (2) | 0.032 (2) | 0.015 (2) |
Cl2 | 0.0381 (13) | 0.0563 (15) | 0.0496 (15) | 0.0048 (10) | 0.0123 (11) | 0.0068 (11) |
O18 | 0.169 (8) | 0.100 (5) | 0.122 (7) | 0.028 (5) | 0.096 (6) | 0.030 (5) |
O19 | 0.051 (5) | 0.059 (6) | 0.211 (16) | 0.000 (5) | −0.007 (7) | 0.070 (8) |
O20 | 0.090 (7) | 0.089 (7) | 0.056 (6) | −0.004 (6) | 0.006 (5) | −0.006 (5) |
O21 | 0.036 (5) | 0.136 (11) | 0.108 (9) | 0.009 (5) | 0.018 (5) | −0.018 (8) |
Cl2A | 0.071 (3) | 0.089 (3) | 0.068 (3) | −0.013 (2) | 0.026 (2) | 0.018 (3) |
O19A | 0.019 (3) | 0.063 (6) | 0.024 (4) | 0.006 (3) | 0.007 (3) | 0.028 (4) |
Geometric parameters (Å, º) top
Nd1—O9 | 2.416 (3) | C3—H3A | 0.9500 |
Nd1—O4Ai | 2.429 (12) | C4—C5 | 1.372 (9) |
Nd1—O4 | 2.456 (12) | C4—C8 | 1.512 (7) |
Nd1—O9i | 2.467 (3) | C5—C6 | 1.410 (7) |
Nd1—O8 | 2.472 (3) | C5—H5A | 0.9500 |
Nd1—O10 | 2.478 (4) | C6—C9 | 1.440 (8) |
Nd1—O3 | 2.484 (4) | C7—H7A | 0.9500 |
Nd1—O11 | 2.512 (3) | C8—H8A | 0.9800 |
Nd1—O2 | 2.546 (3) | C8—H8B | 0.9800 |
Nd1—O5 | 2.565 (3) | C8—H8C | 0.9800 |
Nd1—Nd2 | 3.7019 (4) | C9—H9A | 0.9500 |
Nd1—Nd1i | 3.7376 (5) | C10—C11 | 1.441 (6) |
Nd2—O8 | 2.392 (3) | C10—H10A | 0.9500 |
Nd2—O6 | 2.441 (4) | C11—C13 | 1.415 (7) |
Nd2—O9 | 2.447 (3) | C11—C12 | 1.444 (6) |
Nd2—O1 | 2.452 (3) | C12—C11A | 1.444 (6) |
Nd2—O8i | 2.453 (3) | C13—C14 | 1.382 (7) |
Nd2—O13 | 2.516 (4) | C13—H13A | 0.9500 |
Nd2—O7 | 2.559 (3) | C10A—C11A | 1.440 (6) |
Nd2—O2 | 2.597 (3) | C10A—H10B | 0.9500 |
Nd2—O12 | 2.627 (3) | C11A—C13A | 1.415 (7) |
Nd2—Nd2i | 3.7003 (4) | C13A—C14 | 1.383 (7) |
O1—C7 | 1.228 (6) | C13A—H13B | 0.9500 |
O2—C1 | 1.292 (5) | C14—C15 | 1.515 (13) |
O3—C9 | 1.228 (7) | C15—H15A | 0.9800 |
O4—C10 | 1.227 (6) | C15—H15B | 0.9800 |
O4A—C10A | 1.227 (6) | C15—H15C | 0.9800 |
O4A—Nd1i | 2.429 (12) | C16—C18 | 1.444 (6) |
O5—C12 | 1.276 (7) | C16—H16A | 0.9500 |
O5—C12i | 1.276 (7) | C17—C18 | 1.440 (5) |
O5—Nd1i | 2.565 (3) | C17—C18i | 1.440 (5) |
O6—C16 | 1.227 (6) | C18—C19 | 1.414 (7) |
O7—C17 | 1.276 (7) | C19—C20 | 1.383 (7) |
O7—Nd2i | 2.559 (3) | C19—H19A | 0.9500 |
O8—Nd2i | 2.453 (3) | C20—C19i | 1.383 (7) |
O8—H8 | 1.0000 | C20—C21 | 1.515 (13) |
O9—Nd1i | 2.467 (3) | C21—H21A | 0.9800 |
O9—H9 | 1.0000 | C21—H21B | 0.9800 |
O10—H10C | 0.8399 | C21—H21C | 0.9800 |
O10—H10D | 0.8400 | Cl1—O14 | 1.370 (6) |
O11—H11A | 0.8401 | Cl1—O17 | 1.406 (5) |
O11—H11B | 0.8398 | Cl1—O16 | 1.436 (5) |
O12—H12A | 0.8399 | Cl1—O15 | 1.464 (6) |
O12—H12B | 0.8399 | Cl2—O21 | 1.414 (8) |
O13—H13C | 0.8402 | Cl2—O19 | 1.417 (8) |
O13—H13D | 0.8401 | Cl2—O18 | 1.436 (7) |
C1—C2 | 1.429 (7) | Cl2—O20 | 1.442 (9) |
C1—C6 | 1.431 (7) | O18—Cl2A | 1.505 (9) |
C2—C3 | 1.411 (6) | Cl2A—O20A | 1.440 (14) |
C2—C7 | 1.424 (7) | Cl2A—O21A | 1.458 (15) |
C3—C4 | 1.376 (9) | Cl2A—O19A | 1.563 (8) |
| | | |
O9—Nd1—O4Ai | 133.2 (3) | C12—O5—C12i | 5.1 (7) |
O9—Nd1—O4 | 135.0 (3) | C12—O5—Nd1 | 133.0 (4) |
O4Ai—Nd1—O4 | 7.7 (4) | C12i—O5—Nd1 | 133.3 (4) |
O9—Nd1—O9i | 74.28 (12) | C12—O5—Nd1i | 133.3 (4) |
O4Ai—Nd1—O9i | 102.3 (3) | C12i—O5—Nd1i | 133.0 (4) |
O4—Nd1—O9i | 95.4 (3) | Nd1—O5—Nd1i | 93.56 (16) |
O9—Nd1—O8 | 74.46 (11) | C16—O6—Nd2 | 135.0 (3) |
O4Ai—Nd1—O8 | 147.2 (3) | C17—O7—Nd2 | 133.69 (7) |
O4—Nd1—O8 | 140.6 (3) | C17—O7—Nd2i | 133.69 (7) |
O9i—Nd1—O8 | 64.32 (11) | Nd2—O7—Nd2i | 92.62 (15) |
O9—Nd1—O10 | 144.03 (12) | Nd2—O8—Nd2i | 99.58 (11) |
O4Ai—Nd1—O10 | 75.1 (3) | Nd2—O8—Nd1 | 99.10 (12) |
O4—Nd1—O10 | 69.9 (3) | Nd2i—O8—Nd1 | 115.20 (12) |
O9i—Nd1—O10 | 78.24 (12) | Nd2—O8—H8 | 113.7 |
O8—Nd1—O10 | 72.92 (12) | Nd2i—O8—H8 | 113.7 |
O9—Nd1—O3 | 135.02 (11) | Nd1—O8—H8 | 113.7 |
O4Ai—Nd1—O3 | 70.3 (3) | Nd1—O9—Nd2 | 99.14 (11) |
O4—Nd1—O3 | 74.3 (3) | Nd1—O9—Nd1i | 99.90 (12) |
O9i—Nd1—O3 | 146.66 (12) | Nd2—O9—Nd1i | 115.59 (12) |
O8—Nd1—O3 | 103.70 (12) | Nd1—O9—H9 | 113.5 |
O10—Nd1—O3 | 68.43 (13) | Nd2—O9—H9 | 113.5 |
O9—Nd1—O11 | 79.53 (10) | Nd1i—O9—H9 | 113.5 |
O4Ai—Nd1—O11 | 73.1 (3) | Nd1—O10—H10C | 118.7 |
O4—Nd1—O11 | 80.6 (3) | Nd1—O10—H10D | 124.7 |
O9i—Nd1—O11 | 138.01 (10) | H10C—O10—H10D | 112.0 |
O8—Nd1—O11 | 137.48 (10) | Nd1—O11—H11A | 114.3 |
O10—Nd1—O11 | 135.93 (11) | Nd1—O11—H11B | 92.2 |
O3—Nd1—O11 | 72.60 (12) | H11A—O11—H11B | 121.2 |
O9—Nd1—O2 | 68.39 (11) | Nd2—O12—H12A | 118.5 |
O4Ai—Nd1—O2 | 134.0 (3) | Nd2—O12—H12B | 111.3 |
O4—Nd1—O2 | 140.6 (3) | H12A—O12—H12B | 111.3 |
O9i—Nd1—O2 | 123.73 (11) | Nd2—O13—H13C | 122.0 |
O8—Nd1—O2 | 66.06 (11) | Nd2—O13—H13D | 123.1 |
O10—Nd1—O2 | 110.52 (13) | H13C—O13—H13D | 101.2 |
O3—Nd1—O2 | 70.15 (12) | O2—C1—C2 | 121.5 (4) |
O11—Nd1—O2 | 73.33 (11) | O2—C1—C6 | 122.5 (4) |
O9—Nd1—O5 | 66.45 (10) | C2—C1—C6 | 115.9 (4) |
O4Ai—Nd1—O5 | 69.8 (3) | C3—C2—C7 | 115.1 (5) |
O4—Nd1—O5 | 69.3 (3) | C3—C2—C1 | 120.3 (5) |
O9i—Nd1—O5 | 65.73 (10) | C7—C2—C1 | 124.5 (4) |
O8—Nd1—O5 | 122.64 (11) | C4—C3—C2 | 123.1 (5) |
O10—Nd1—O5 | 121.37 (11) | C4—C3—H3A | 118.4 |
O3—Nd1—O5 | 133.64 (13) | C2—C3—H3A | 118.4 |
O11—Nd1—O5 | 73.94 (8) | C5—C4—C3 | 117.2 (5) |
O2—Nd1—O5 | 127.76 (8) | C5—C4—C8 | 121.8 (6) |
O9—Nd1—Nd2 | 40.75 (8) | C3—C4—C8 | 121.1 (6) |
O4Ai—Nd1—Nd2 | 173.1 (3) | C4—C5—C6 | 122.9 (5) |
O4—Nd1—Nd2 | 174.3 (3) | C4—C5—H5A | 118.5 |
O9i—Nd1—Nd2 | 79.90 (7) | C6—C5—H5A | 118.5 |
O8—Nd1—Nd2 | 39.65 (7) | C5—C6—C1 | 120.5 (5) |
O10—Nd1—Nd2 | 111.89 (10) | C5—C6—C9 | 114.6 (5) |
O3—Nd1—Nd2 | 111.46 (9) | C1—C6—C9 | 124.8 (5) |
O11—Nd1—Nd2 | 100.79 (7) | O1—C7—C2 | 128.2 (5) |
O2—Nd1—Nd2 | 44.51 (7) | O1—C7—H7A | 115.9 |
O5—Nd1—Nd2 | 105.57 (7) | C2—C7—H7A | 115.9 |
O9—Nd1—Nd1i | 40.56 (7) | C4—C8—H8A | 109.5 |
O4Ai—Nd1—Nd1i | 109.5 (3) | C4—C8—H8B | 109.5 |
O4—Nd1—Nd1i | 106.3 (3) | H8A—C8—H8B | 109.5 |
O9i—Nd1—Nd1i | 39.55 (7) | C4—C8—H8C | 109.5 |
O8—Nd1—Nd1i | 79.88 (7) | H8A—C8—H8C | 109.5 |
O10—Nd1—Nd1i | 117.74 (9) | H8B—C8—H8C | 109.5 |
O3—Nd1—Nd1i | 173.74 (10) | O3—C9—C6 | 128.1 (5) |
O11—Nd1—Nd1i | 101.26 (6) | O3—C9—H9A | 115.9 |
O2—Nd1—Nd1i | 107.26 (7) | C6—C9—H9A | 115.9 |
O5—Nd1—Nd1i | 43.22 (8) | O4—C10—C11 | 137.0 (18) |
Nd2—Nd1—Nd1i | 67.960 (6) | O4—C10—H10A | 111.5 |
O8—Nd2—O6 | 133.98 (12) | C11—C10—H10A | 111.5 |
O8—Nd2—O9 | 75.33 (11) | C13—C11—C10 | 121.1 (11) |
O6—Nd2—O9 | 143.45 (12) | C13—C11—C12 | 120.8 (10) |
O8—Nd2—O1 | 133.04 (11) | C10—C11—C12 | 118.0 (13) |
O6—Nd2—O1 | 76.66 (12) | O5—C12—C11A | 123.3 (8) |
O9—Nd2—O1 | 98.62 (12) | O5—C12—C11 | 122.1 (9) |
O8—Nd2—O8i | 75.01 (12) | C11A—C12—C11 | 113.5 (7) |
O6—Nd2—O8i | 98.18 (12) | C14—C13—C11 | 123.8 (13) |
O9—Nd2—O8i | 64.89 (11) | C14—C13—H13A | 118.1 |
O1—Nd2—O8i | 145.01 (12) | C11—C13—H13A | 118.1 |
O8—Nd2—O13 | 82.05 (13) | O4A—C10A—C11A | 126.2 (14) |
O6—Nd2—O13 | 73.86 (14) | O4A—C10A—H10B | 116.9 |
O9—Nd2—O13 | 140.48 (12) | C11A—C10A—H10B | 116.9 |
O1—Nd2—O13 | 73.95 (14) | C13A—C11A—C10A | 112.5 (10) |
O8i—Nd2—O13 | 138.63 (12) | C13A—C11A—C12 | 123.5 (11) |
O8—Nd2—O7 | 66.61 (10) | C10A—C11A—C12 | 124.1 (12) |
O6—Nd2—O7 | 69.20 (10) | C14—C13A—C11A | 121.1 (14) |
O9—Nd2—O7 | 123.36 (10) | C14—C13A—H13B | 119.5 |
O1—Nd2—O7 | 138.02 (12) | C11A—C13A—H13B | 119.5 |
O8i—Nd2—O7 | 65.76 (9) | C13—C14—C13A | 117.4 (15) |
O13—Nd2—O7 | 73.67 (11) | C13—C14—C15 | 121.3 (8) |
O8—Nd2—O2 | 66.36 (11) | C13A—C14—C15 | 121.3 (8) |
O6—Nd2—O2 | 137.84 (12) | O6—C16—C18 | 127.4 (5) |
O9—Nd2—O2 | 67.10 (11) | O6—C16—H16A | 116.3 |
O1—Nd2—O2 | 68.50 (11) | C18—C16—H16A | 116.3 |
O8i—Nd2—O2 | 123.97 (11) | O7—C17—C18 | 122.4 (3) |
O13—Nd2—O2 | 74.27 (13) | O7—C17—C18i | 122.4 (3) |
O7—Nd2—O2 | 125.60 (8) | C18—C17—C18i | 115.2 (6) |
O8—Nd2—O12 | 146.21 (10) | C19—C18—C17 | 120.9 (5) |
O6—Nd2—O12 | 69.45 (11) | C19—C18—C16 | 115.2 (5) |
O9—Nd2—O12 | 75.19 (10) | C17—C18—C16 | 123.8 (5) |
O1—Nd2—O12 | 67.92 (11) | C20—C19—C18 | 123.0 (6) |
O8i—Nd2—O12 | 77.80 (9) | C20—C19—H19A | 118.5 |
O13—Nd2—O12 | 131.68 (12) | C18—C19—H19A | 118.5 |
O7—Nd2—O12 | 118.72 (6) | C19—C20—C19i | 117.1 (8) |
O2—Nd2—O12 | 115.50 (10) | C19—C20—C21 | 121.5 (4) |
O8—Nd2—Nd2i | 40.82 (7) | C19i—C20—C21 | 121.5 (4) |
O6—Nd2—Nd2i | 107.94 (8) | C20—C21—H21A | 109.5 |
O9—Nd2—Nd2i | 80.16 (7) | C20—C21—H21B | 109.5 |
O1—Nd2—Nd2i | 173.85 (8) | H21A—C21—H21B | 109.5 |
O8i—Nd2—Nd2i | 39.61 (7) | C20—C21—H21C | 109.5 |
O13—Nd2—Nd2i | 103.11 (10) | H21A—C21—H21C | 109.5 |
O7—Nd2—Nd2i | 43.69 (7) | H21B—C21—H21C | 109.5 |
O2—Nd2—Nd2i | 105.60 (7) | O14—Cl1—O17 | 111.1 (4) |
O12—Nd2—Nd2i | 117.26 (6) | O14—Cl1—O16 | 112.0 (5) |
O8—Nd2—Nd1 | 41.25 (8) | O17—Cl1—O16 | 110.9 (3) |
O6—Nd2—Nd1 | 175.23 (8) | O14—Cl1—O15 | 110.5 (7) |
O9—Nd2—Nd1 | 40.11 (7) | O17—Cl1—O15 | 106.6 (4) |
O1—Nd2—Nd1 | 106.83 (9) | O16—Cl1—O15 | 105.2 (4) |
O8i—Nd2—Nd1 | 80.85 (8) | O21—Cl2—O19 | 112.7 (7) |
O13—Nd2—Nd1 | 103.75 (10) | O21—Cl2—O18 | 107.7 (7) |
O7—Nd2—Nd1 | 106.25 (6) | O19—Cl2—O18 | 113.7 (9) |
O2—Nd2—Nd1 | 43.41 (7) | O21—Cl2—O20 | 109.6 (8) |
O12—Nd2—Nd1 | 114.73 (7) | O19—Cl2—O20 | 102.1 (8) |
Nd2i—Nd2—Nd1 | 68.352 (6) | O18—Cl2—O20 | 111.0 (7) |
C7—O1—Nd2 | 135.8 (3) | Cl2—O18—Cl2A | 117.7 (6) |
C1—O2—Nd1 | 134.4 (3) | O20A—Cl2A—O21A | 105.5 (18) |
C1—O2—Nd2 | 133.6 (3) | O20A—Cl2A—O18 | 111.2 (12) |
Nd1—O2—Nd2 | 92.08 (10) | O21A—Cl2A—O18 | 112.8 (14) |
C9—O3—Nd1 | 135.6 (4) | O20A—Cl2A—O19A | 92.1 (12) |
C10—O4—Nd1 | 122.6 (10) | O21A—Cl2A—O19A | 110.4 (14) |
C10A—O4A—Nd1i | 139.4 (11) | O18—Cl2A—O19A | 121.9 (6) |
Symmetry code: (i) −x, y, −z+1/2. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O8—H8···O19i | 1.00 | 1.98 | 2.969 (10) | 168 |
O9—H9···O15i | 1.00 | 1.93 | 2.922 (7) | 170 |
O10—H10C···O3ii | 0.84 | 2.05 | 2.884 (5) | 170 |
O10—H10D···O12i | 0.84 | 1.98 | 2.764 (5) | 155 |
O11—H11A···O14i | 0.84 | 2.49 | 3.331 (14) | 180 |
O12—H12A···O19A | 0.84 | 2.10 | 2.945 (8) | 180 |
O12—H12B···O16i | 0.84 | 1.98 | 2.819 (6) | 180 |
O13—H13C···O20i | 0.84 | 2.01 | 2.845 (12) | 180 |
O13—H13D···O19Aiii | 0.84 | 2.10 | 2.943 (8) | 180 |
Symmetry codes: (i) −x, y, −z+1/2; (ii) −x−1/2, −y+1/2, −z; (iii) −x, −y, −z+1. |
Experimental details
Crystal data |
Chemical formula | [Nd4(C9H7O3)4(OH)4(H2O)8](ClO4)4·2C2H6O |
Mr | 1931.64 |
Crystal system, space group | Monoclinic, C2/c |
Temperature (K) | 150 |
a, b, c (Å) | 20.9933 (3), 24.7385 (5), 17.6893 (3) |
β (°) | 120.469 (1) |
V (Å3) | 7918.1 (2) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 2.80 |
Crystal size (mm) | 0.32 × 0.28 × 0.25 |
|
Data collection |
Diffractometer | Bruker Nonius KappaCCD area detector diffractometer |
Absorption correction | Multi-scan (DENZO-SMN; Otwinowski & Minor, 1997) |
Tmin, Tmax | 0.430, 0.497 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 31251, 8998, 7708 |
Rint | 0.037 |
(sin θ/λ)max (Å−1) | 0.649 |
|
Refinement |
R[F2 > 2σ(F2)], wR(F2), S | 0.043, 0.122, 1.06 |
No. of reflections | 8998 |
No. of parameters | 400 |
No. of restraints | 55 |
H-atom treatment | H-atom parameters constrained |
| w = 1/[σ2(Fo2) + (0.0625P)2 + 41.2001P] where P = (Fo2 + 2Fc2)/3 |
Δρmax, Δρmin (e Å−3) | 1.64, −1.16 |
Selected bond lengths (Å) topNd1—O9 | 2.416 (3) | Nd2—O8 | 2.392 (3) |
Nd1—O4Ai | 2.429 (12) | Nd2—O6 | 2.441 (4) |
Nd1—O4 | 2.456 (12) | Nd2—O9 | 2.447 (3) |
Nd1—O9i | 2.467 (3) | Nd2—O1 | 2.452 (3) |
Nd1—O8 | 2.472 (3) | Nd2—O8i | 2.453 (3) |
Nd1—O10 | 2.478 (4) | Nd2—O13 | 2.516 (4) |
Nd1—O3 | 2.484 (4) | Nd2—O7 | 2.559 (3) |
Nd1—O11 | 2.512 (3) | Nd2—O2 | 2.597 (3) |
Nd1—O2 | 2.546 (3) | Nd2—O12 | 2.627 (3) |
Nd1—O5 | 2.565 (3) | | |
Symmetry code: (i) −x, y, −z+1/2. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O8—H8···O19i | 1.00 | 1.98 | 2.969 (10) | 168 |
O9—H9···O15i | 1.00 | 1.93 | 2.922 (7) | 170 |
O10—H10C···O3ii | 0.84 | 2.05 | 2.884 (5) | 170 |
O10—H10D···O12i | 0.84 | 1.98 | 2.764 (5) | 155 |
O11—H11A···O14i | 0.84 | 2.49 | 3.331 (14) | 180 |
O12—H12A···O19A | 0.84 | 2.10 | 2.945 (8) | 180 |
O12—H12B···O16i | 0.84 | 1.98 | 2.819 (6) | 180 |
O13—H13C···O20i | 0.84 | 2.01 | 2.845 (12) | 180 |
O13—H13D···O19Aiii | 0.84 | 2.10 | 2.943 (8) | 180 |
Symmetry codes: (i) −x, y, −z+1/2; (ii) −x−1/2, −y+1/2, −z; (iii) −x, −y, −z+1. |
There is currently tremendous interest in the synthesis and characterization of finite polylanthanide(III) entities with nanoscopic dimensions (Zheng, 2001; Wang et al., 2002). This interest lies in several application fields, since lanthanide clusters are potential precurors for ceramics, catalysts and thin-film coatings (Hubert-Pfalzgraf, 1995). Nanoclusters with mutually interacting LnIII ions are also expected to yield new materials with greater versatility resulting from unusual enhancements in magnetic, catalytic, optical and electronic properties (Thompson et al., 2003, 2001). The title compound, (I), is one of a series of similar LnIII compounds synthesized in an investigation into the formation chemistry of nanoclusters which feature commonly encountered aggregation motifs such as [Ln4(OH)4]8+. We have previously determined the structure of the cation in the title structure as the trifluoromethanesulfonate (Singh-Wilmot et al., 2005).
The cation in (I) features four NdIII and four µ3-hydroxo groups occupying alternate vertices of a distorted cube (Fig. 1). Selected bond distances are given in Table 1. Each NdIII ion is in a ninefold coordination polyhedron of an approximate tricapped trigonal prism and approximate D3 h symmetry, with a shortest metal–metal contact of Nd2···Nd2i = 3.7003 (4) Å [symmetry code: (i) −x, y, 1/2 − z]. This distance is comparable with metal–metal distances seen in other complexes containing a similar cubane-type [Ln4(µ3-OH)4]8+ core, for example ca 3.83 Å for the shortest Sm···Sm distance in [Sm4(µ3-OH)4(Gly)5(H2O)11]) (Evans et al., 2000). Nd—O(phenolate) distances are in the range 2.546 (3)–2.597 (3) Å, while the Nd—O(carbonyl) distances are in the range 2.441 (4)–2.484 (4) Å. The range of Nd—O(µ3-OH) distances [2.393 (3)–2.472 (3) Å] compares well with those in [Nd4(µ3-OH)4(Ala)6(H2O)10] (ca 2.43 Å; Zheng & Wang, 2000).