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The title compound, [Nd4(μ3-OH)4(μ2-C9H7O3)4(H2O)8](CF3SO3)4·2C4H10O·4H2O, was synthesized from Nd(CF3SO3)3 and 2,6-diformyl-4-methylphenol at relatively high pH. The cation, which lies on a crystallographic twofold axis, features a cubane-type [Ln4(OH)4]8+ core of four NdIII cations and four μ3-OH ligands occupying alternate vertices of a distorted cube.
Supporting information
CCDC reference: 271882
Key indicators
- Single-crystal X-ray study
- T = 150 K
- Mean (C-C) = 0.010 Å
Some non-H atoms missing
- Disorder in solvent or counterion
- R factor = 0.049
- wR factor = 0.122
- Data-to-parameter ratio = 19.9
checkCIF/PLATON results
No syntax errors found
Alert level A
PLAT220_ALERT_2_A Large Non-Solvent C Ueq(max)/Ueq(min) ... 5.00 Ratio
| Author Response: Atom C8 and the bonded H atoms consitute the terminal methyl
group of the coordinated 2,6-diformyl-4-methylphenol ligand. The
dispacement ellipsoids of these atoms indicate that these atoms may be
disordered. Attempts were made to construct a disorder model but the
'split' atoms also showed unusually large displacement ellipsoids. In the
final cycles of the refinement the atom C8 was refined as full occupancy
the large displacement of this atom has been interpreted as dynamic
disorder and the anisotropic model is expected to be sufficient.
|
PLAT222_ALERT_3_A Large Non-Solvent H Ueq(max)/Ueq(min) ... 6.88 Ratio
| Author Response: (see above)
|
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 2258.29
TEST: Calculate formula weight from _atom_site_*
atom mass num sum
C 12.01 40.00 480.44
H 1.01 56.00 56.45
O 16.00 40.00 639.96
F 19.00 12.00 227.98
S 32.07 4.00 128.26
Nd 144.24 4.00 576.96
Calculated formula weight 2110.05
PLAT043_ALERT_1_B Check Reported Molecular Weight ................ 2258.29
| Author Response: (see experimental text)
|
PLAT044_ALERT_1_B Calculated and Reported Dx Differ .............. ?
| Author Response: (see experimental text)
|
PLAT416_ALERT_2_B Short Intra D-H..H-D H11E .. H13D .. 1.87 Ang.
| Author Response: The H atoms bonded to the O atoms of the coordinated and
solvent water atoms were not visible in differnce Fourier maps. The
final positions of these H atoms were based on the most likely location
for these atoms to be involved in O-H...O hydrogen bonding (see Table 2.
in the manuscript). The H atom positions were idealized so that the O-H
distances were 0.84\% and the O-H...O angle was close to 180\%; the
exact O-H...O angles are probably less the 180\%. The idealized positions
for the H atoms is reflected in the close intermolecular distances.
|
PLAT417_ALERT_2_B Short Inter D-H..H-D H1WB .. H11D .. 2.03 Ang.
| Author Response: (see above)
|
PLAT417_ALERT_2_B Short Inter D-H..H-D H1WB .. H10E .. 1.84 Ang.
| Author Response: (see above)
|
PLAT417_ALERT_2_B Short Inter D-H..H-D H2WA .. H13E .. 1.99 Ang.
| Author Response: (see above)
|
PLAT417_ALERT_2_B Short Inter D-H..H-D H2WB .. H13E .. 1.94 Ang.
| Author Response: (see above)
|
PLAT417_ALERT_2_B Short Inter D-H..H-D H2WB .. H12E .. 1.80 Ang.
| Author Response: (see above)
|
PLAT420_ALERT_2_B D-H Without Acceptor O1W - H1WB ... ?
| Author Response: O1W-H1WB and O2W-H2WB are invloved in O-H...\p interations
(see Table 2 in the manuscript)
|
Alert level C
PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings Differ .... ?
PLAT068_ALERT_1_C Reported F000 Differs from Calcd (or Missing)... ?
PLAT213_ALERT_2_C Atom C8 has ADP max/min Ratio ............. 4.00 prolat
PLAT213_ALERT_2_C Atom C21 has ADP max/min Ratio ............. 3.80 prolat
PLAT244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for S1
PLAT244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for C22
PLAT302_ALERT_4_C Anion/Solvent Disorder ......................... 22.00 Perc.
PLAT342_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 11
PLAT602_ALERT_4_C VERY LARGE Solvent Accessible VOID(S) in Structure !
| Author Response: (see experimental text)
|
PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 9
PLAT764_ALERT_4_C Overcomplete CIF Bond List Detected (Rep/Expd) . 1.17 Ratio
PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 4
H2 O
PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 5
H2 O
Alert level G
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:C48 H76 F12 Nd4 O42 S4
Atom count from the _atom_site data: C40 H56 F12 Nd4 O40 S4
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 C48 H76 F12 Nd4 O42 S4
TEST: Compare cell contents of formula and atom_site data
atom Z*formula cif sites diff
C 192.00 160.00 32.00
H 304.00 224.00 80.00
F 48.00 48.00 0.00
Nd 16.00 16.00 0.00
O 168.00 160.00 8.00
S 16.00 16.00 0.00
2 ALERT level A = In general: serious problem
10 ALERT level B = Potentially serious problem
13 ALERT level C = Check and explain
3 ALERT level G = General alerts; check
6 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
8 ALERT type 4 Improvement, methodology, query or suggestion
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.
Crystal data top
[Nd4(OH)4(C9H7O3)4(H2O)8](CF3SO3)4·2C4H10O·4H2O | F(000) = 4448 |
Mr = 2258.29 | Dx = 1.700 Mg m−3 |
Monoclinic, C2/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -C 2yc | Cell parameters from 38049 reflections |
a = 24.0937 (4) Å | θ = 2.6–27.5° |
b = 24.6345 (5) Å | µ = 2.52 mm−1 |
c = 16.7428 (3) Å | T = 150 K |
β = 117.3750 (11)° | Cube, yellow |
V = 8824.6 (3) Å3 | 0.32 × 0.28 × 0.26 mm |
Z = 4 | |
Data collection top
Nonius KappaCCD diffractometer | 10085 independent reflections |
Radiation source: fine-focus sealed tube | 9158 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.055 |
Detector resolution: 9 pixels mm-1 | θmax = 27.5°, θmin = 2.7° |
φ scans and ω scans with κ offsets | h = −31→27 |
Absorption correction: multi-scan (SORTAV; Blessing 1995) | k = −31→31 |
Tmin = 0.456, Tmax = 0.517 | l = −21→21 |
38049 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)] = 0.049 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.122 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.23 | w = 1/[σ2(Fo2) + 141.614P] where P = (Fo2 + 2Fc2)/3 |
10085 reflections | (Δ/σ)max < 0.001 |
508 parameters | Δρmax = 1.38 e Å−3 |
58 restraints | Δρmin = −1.31 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 | 0.465265 (13) | 0.106654 (12) | 0.329472 (19) | 0.01938 (8) | |
Nd2 | 0.414212 (13) | 0.224031 (12) | 0.171313 (19) | 0.01993 (8) | |
O1 | 0.41068 (19) | 0.1173 (2) | 0.4241 (3) | 0.0307 (10) | |
O2 | 0.36632 (18) | 0.16249 (17) | 0.2496 (3) | 0.0244 (8) | |
O3 | 0.30016 (19) | 0.21278 (18) | 0.0801 (3) | 0.0282 (9) | |
O4 | 0.3907 (2) | 0.30838 (18) | 0.0826 (3) | 0.0314 (10) | |
O5 | 0.5000 | 0.2967 (2) | 0.2500 | 0.0236 (12) | |
O6 | 0.5110 (2) | 0.02559 (18) | 0.4235 (3) | 0.0289 (9) | |
O7 | 0.5000 | 0.0363 (2) | 0.2500 | 0.0236 (12) | |
O8 | 0.48634 (17) | 0.20369 (16) | 0.3269 (3) | 0.0204 (8) | |
H8O | 0.477 (3) | 0.221 (3) | 0.362 (4) | 0.024* | |
O9 | 0.43744 (17) | 0.12800 (16) | 0.1749 (3) | 0.0201 (8) | |
H9O | 0.408 (3) | 0.107 (3) | 0.147 (4) | 0.024* | |
O10 | 0.3660 (2) | 0.28682 (18) | 0.2375 (3) | 0.0316 (10) | |
H10D | 0.3921 | 0.2870 | 0.2922 | 0.038* | |
H10E | 0.3300 | 0.2990 | 0.2048 | 0.038* | |
O11 | 0.3805 (2) | 0.2050 (2) | 0.0054 (3) | 0.0394 (12) | |
H11D | 0.3444 | 0.1956 | −0.0328 | 0.047* | |
H11E | 0.4025 | 0.2229 | −0.0122 | 0.047* | |
O12 | 0.3815 (2) | 0.03633 (19) | 0.2783 (3) | 0.0353 (10) | |
H12D | 0.3501 | 0.0372 | 0.2275 | 0.042* | |
H12E | 0.3808 | 0.0108 | 0.3111 | 0.042* | |
O13 | 0.5386 (2) | 0.1293 (2) | 0.4943 (3) | 0.0397 (12) | |
H13D | 0.5637 | 0.1530 | 0.4945 | 0.048* | |
H13E | 0.5628 | 0.1057 | 0.5291 | 0.048* | |
C1 | 0.3569 (3) | 0.1282 (3) | 0.4100 (5) | 0.0325 (14) | |
H1A | 0.3482 | 0.1235 | 0.4594 | 0.039* | |
C2 | 0.3059 (3) | 0.1473 (3) | 0.3277 (4) | 0.0322 (14) | |
C3 | 0.2481 (3) | 0.1506 (4) | 0.3272 (5) | 0.052 (2) | |
H3A | 0.2460 | 0.1416 | 0.3809 | 0.062* | |
C4 | 0.1937 (4) | 0.1661 (5) | 0.2532 (6) | 0.066 (3) | |
C5 | 0.1994 (3) | 0.1816 (4) | 0.1774 (5) | 0.051 (2) | |
H5A | 0.1627 | 0.1920 | 0.1250 | 0.061* | |
C6 | 0.2567 (3) | 0.1827 (3) | 0.1750 (4) | 0.0333 (14) | |
C7 | 0.3132 (2) | 0.1641 (3) | 0.2512 (4) | 0.0241 (12) | |
C8 | 0.1310 (4) | 0.1664 (7) | 0.2557 (8) | 0.110 (6) | |
H8A | 0.1085 | 0.1326 | 0.2297 | 0.165* | |
H8B | 0.1059 | 0.1973 | 0.2209 | 0.165* | |
H8C | 0.1383 | 0.1696 | 0.3182 | 0.165* | |
C9 | 0.2548 (3) | 0.2027 (3) | 0.0939 (4) | 0.0297 (13) | |
H9A | 0.2145 | 0.2091 | 0.0453 | 0.036* | |
C10 | 0.4050 (3) | 0.3568 (3) | 0.0964 (4) | 0.0297 (13) | |
H10A | 0.3811 | 0.3811 | 0.0488 | 0.036* | |
C11 | 0.4538 (3) | 0.3808 (2) | 0.1767 (4) | 0.0282 (13) | |
C12 | 0.4559 (3) | 0.4373 (3) | 0.1782 (5) | 0.0351 (15) | |
H12A | 0.4256 | 0.4565 | 0.1277 | 0.042* | |
C13 | 0.5000 | 0.4675 (4) | 0.2500 | 0.037 (2) | |
C14 | 0.5000 | 0.3492 (3) | 0.2500 | 0.0224 (16) | |
C15 | 0.5000 | 0.5289 (4) | 0.2500 | 0.052 (3) | |
H15A | 0.5348 | 0.5421 | 0.3057 | 0.078* | 0.50 |
H15B | 0.4605 | 0.5421 | 0.2461 | 0.078* | 0.50 |
H15C | 0.5047 | 0.5421 | 0.1982 | 0.078* | 0.50 |
C16 | 0.5184 (3) | −0.0225 (3) | 0.4109 (4) | 0.0318 (14) | |
H16A | 0.5312 | −0.0460 | 0.4613 | 0.038* | |
C17 | 0.5097 (3) | −0.0473 (3) | 0.3271 (4) | 0.0313 (13) | |
C18 | 0.5119 (4) | −0.1043 (3) | 0.3262 (5) | 0.0454 (19) | |
H18A | 0.5220 | −0.1236 | 0.3803 | 0.054* | |
C19 | 0.5000 | −0.1329 (4) | 0.2500 | 0.066 (4) | |
C20 | 0.5000 | −0.0162 (4) | 0.2500 | 0.0267 (17) | |
C21 | 0.5000 | −0.1949 (5) | 0.2500 | 0.093 (6) | |
H21A | 0.4909 | −0.2081 | 0.1900 | 0.139* | 0.50 |
H21B | 0.4680 | −0.2081 | 0.2659 | 0.139* | 0.50 |
H21C | 0.5411 | −0.2081 | 0.2941 | 0.139* | 0.50 |
S1 | 0.27660 (7) | 0.05256 (7) | 0.02594 (11) | 0.0335 (3) | |
F1 | 0.2857 (5) | −0.0507 (3) | 0.0067 (7) | 0.134 (3) | |
F2 | 0.2517 (4) | −0.0065 (4) | −0.1148 (5) | 0.122 (3) | |
F3 | 0.1926 (3) | −0.0224 (3) | −0.0528 (5) | 0.097 (2) | |
O14 | 0.2304 (3) | 0.0915 (3) | −0.0271 (4) | 0.0572 (16) | |
O15 | 0.3376 (2) | 0.0613 (3) | 0.0325 (4) | 0.0483 (13) | |
O16 | 0.2768 (2) | 0.0391 (2) | 0.1094 (3) | 0.0476 (13) | |
C22 | 0.2486 (5) | −0.0078 (4) | −0.0394 (7) | 0.070 (3) | |
S2 | 0.49436 (19) | 0.30529 (19) | 0.5037 (3) | 0.0431 (12) | 0.470 (5) |
F4 | 0.4167 (6) | 0.2663 (5) | 0.5576 (9) | 0.074 (4) | 0.470 (5) |
F5 | 0.4773 (2) | 0.3185 (2) | 0.6485 (3) | 0.0601 (14) | |
F6 | 0.4036 (2) | 0.3496 (2) | 0.5246 (4) | 0.0665 (15) | |
O17 | 0.5174 (7) | 0.3595 (5) | 0.5084 (11) | 0.071 (4) | 0.470 (5) |
O18 | 0.4507 (6) | 0.2874 (7) | 0.4154 (7) | 0.057 (4) | 0.470 (5) |
O19 | 0.5423 (5) | 0.2678 (5) | 0.5570 (7) | 0.049 (3) | 0.470 (5) |
C23 | 0.4504 (3) | 0.3158 (3) | 0.5628 (5) | 0.052 (2) | |
S2* | 0.43943 (16) | 0.25077 (15) | 0.5094 (2) | 0.0408 (10) | 0.530 (5) |
F4* | 0.4975 (5) | 0.3441 (5) | 0.5492 (8) | 0.075 (3) | 0.530 (5) |
O17* | 0.3889 (5) | 0.2310 (5) | 0.5244 (9) | 0.063 (3) | 0.530 (5) |
O18* | 0.4238 (6) | 0.2631 (5) | 0.4173 (6) | 0.048 (3) | 0.530 (5) |
O19* | 0.4972 (4) | 0.2230 (4) | 0.5565 (6) | 0.043 (2) | 0.530 (5) |
O1W | 0.2548 (2) | 0.1721 (2) | −0.1290 (3) | 0.0386 (11) | |
H1WA | 0.2476 | 0.1483 | −0.0990 | 0.046* | |
H1WB | 0.2523 | 0.2053 | −0.1198 | 0.046* | |
O2W | 0.3784 (2) | 0.0492 (2) | −0.1131 (3) | 0.0474 (13) | |
H2WA | 0.3670 | 0.0526 | −0.0729 | 0.057* | |
H2WB | 0.4143 | 0.0424 | −0.1071 | 0.057* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Nd1 | 0.01678 (14) | 0.02186 (15) | 0.01841 (15) | −0.00153 (10) | 0.00715 (11) | 0.00088 (11) |
Nd2 | 0.01595 (14) | 0.02105 (15) | 0.01945 (15) | 0.00272 (10) | 0.00529 (11) | 0.00145 (11) |
O1 | 0.021 (2) | 0.046 (3) | 0.026 (2) | 0.0061 (18) | 0.0123 (17) | 0.008 (2) |
O2 | 0.0186 (18) | 0.030 (2) | 0.025 (2) | 0.0030 (16) | 0.0104 (16) | 0.0025 (17) |
O3 | 0.020 (2) | 0.035 (2) | 0.024 (2) | 0.0004 (17) | 0.0063 (17) | 0.0032 (18) |
O4 | 0.030 (2) | 0.026 (2) | 0.029 (2) | 0.0009 (17) | 0.0059 (18) | 0.0055 (18) |
O5 | 0.018 (3) | 0.021 (3) | 0.027 (3) | 0.000 | 0.007 (2) | 0.000 |
O6 | 0.032 (2) | 0.029 (2) | 0.022 (2) | 0.0037 (18) | 0.0095 (18) | 0.0052 (17) |
O7 | 0.027 (3) | 0.021 (3) | 0.022 (3) | 0.000 | 0.010 (2) | 0.000 |
O8 | 0.0133 (17) | 0.025 (2) | 0.023 (2) | 0.0011 (14) | 0.0087 (15) | −0.0025 (16) |
O9 | 0.0171 (18) | 0.0220 (19) | 0.0213 (19) | −0.0051 (15) | 0.0091 (15) | −0.0036 (15) |
O10 | 0.027 (2) | 0.034 (2) | 0.030 (2) | 0.0104 (18) | 0.0099 (18) | −0.0001 (19) |
O11 | 0.029 (2) | 0.042 (3) | 0.032 (2) | 0.011 (2) | 0.0001 (19) | −0.009 (2) |
O12 | 0.032 (2) | 0.035 (2) | 0.032 (2) | −0.0095 (19) | 0.0084 (19) | 0.002 (2) |
O13 | 0.029 (2) | 0.053 (3) | 0.029 (2) | −0.013 (2) | 0.0062 (19) | 0.008 (2) |
C1 | 0.025 (3) | 0.043 (4) | 0.035 (3) | 0.000 (3) | 0.018 (3) | 0.001 (3) |
C2 | 0.020 (3) | 0.045 (4) | 0.033 (3) | 0.005 (3) | 0.014 (3) | 0.009 (3) |
C3 | 0.026 (3) | 0.094 (7) | 0.042 (4) | 0.005 (4) | 0.022 (3) | 0.015 (4) |
C4 | 0.023 (4) | 0.129 (9) | 0.051 (5) | 0.013 (5) | 0.019 (3) | 0.017 (5) |
C5 | 0.018 (3) | 0.092 (7) | 0.041 (4) | 0.003 (4) | 0.014 (3) | 0.009 (4) |
C6 | 0.017 (3) | 0.050 (4) | 0.033 (3) | 0.005 (3) | 0.011 (2) | 0.000 (3) |
C7 | 0.012 (2) | 0.035 (3) | 0.025 (3) | 0.000 (2) | 0.009 (2) | −0.001 (2) |
C8 | 0.026 (4) | 0.240 (18) | 0.075 (7) | 0.013 (7) | 0.032 (5) | 0.028 (9) |
C9 | 0.022 (3) | 0.031 (3) | 0.026 (3) | 0.004 (2) | 0.002 (2) | −0.003 (2) |
C10 | 0.025 (3) | 0.027 (3) | 0.033 (3) | 0.002 (2) | 0.011 (3) | 0.007 (3) |
C11 | 0.029 (3) | 0.022 (3) | 0.033 (3) | 0.003 (2) | 0.014 (3) | 0.004 (2) |
C12 | 0.039 (4) | 0.023 (3) | 0.044 (4) | 0.006 (3) | 0.019 (3) | 0.008 (3) |
C13 | 0.043 (5) | 0.018 (4) | 0.050 (6) | 0.000 | 0.022 (5) | 0.000 |
C14 | 0.019 (4) | 0.020 (4) | 0.027 (4) | 0.000 | 0.010 (3) | 0.000 |
C15 | 0.058 (7) | 0.016 (4) | 0.076 (8) | 0.000 | 0.026 (6) | 0.000 |
C16 | 0.030 (3) | 0.032 (3) | 0.030 (3) | 0.001 (3) | 0.012 (3) | 0.009 (3) |
C17 | 0.036 (3) | 0.025 (3) | 0.029 (3) | −0.004 (2) | 0.012 (3) | 0.005 (3) |
C18 | 0.062 (5) | 0.027 (3) | 0.038 (4) | −0.006 (3) | 0.015 (4) | 0.005 (3) |
C19 | 0.091 (10) | 0.017 (5) | 0.058 (8) | 0.000 | 0.008 (7) | 0.000 |
C20 | 0.025 (4) | 0.025 (4) | 0.027 (4) | 0.000 | 0.009 (3) | 0.000 |
C21 | 0.152 (17) | 0.014 (5) | 0.070 (10) | 0.000 | 0.014 (10) | 0.000 |
S1 | 0.0255 (7) | 0.0373 (9) | 0.0326 (8) | −0.0020 (6) | 0.0089 (6) | −0.0004 (7) |
F1 | 0.168 (9) | 0.060 (4) | 0.163 (9) | 0.023 (5) | 0.068 (7) | −0.030 (5) |
F2 | 0.137 (7) | 0.168 (8) | 0.095 (5) | −0.080 (6) | 0.080 (5) | −0.083 (6) |
F3 | 0.086 (4) | 0.108 (5) | 0.092 (5) | −0.067 (4) | 0.036 (4) | −0.045 (4) |
O14 | 0.038 (3) | 0.063 (4) | 0.066 (4) | 0.011 (3) | 0.020 (3) | 0.022 (3) |
O15 | 0.025 (2) | 0.072 (4) | 0.043 (3) | −0.005 (2) | 0.011 (2) | −0.008 (3) |
O16 | 0.040 (3) | 0.061 (4) | 0.035 (3) | −0.013 (2) | 0.011 (2) | 0.001 (2) |
C22 | 0.074 (7) | 0.068 (7) | 0.071 (7) | −0.021 (5) | 0.035 (6) | −0.026 (5) |
S2 | 0.042 (2) | 0.058 (3) | 0.0305 (19) | 0.0167 (18) | 0.0175 (16) | −0.0036 (18) |
F4 | 0.066 (8) | 0.091 (10) | 0.080 (9) | −0.013 (7) | 0.044 (7) | 0.006 (8) |
F5 | 0.056 (3) | 0.084 (4) | 0.037 (2) | 0.015 (3) | 0.018 (2) | −0.010 (2) |
F6 | 0.057 (3) | 0.068 (3) | 0.065 (3) | 0.033 (3) | 0.020 (3) | 0.005 (3) |
O17 | 0.084 (11) | 0.067 (10) | 0.080 (11) | −0.014 (8) | 0.053 (9) | −0.015 (8) |
O18 | 0.047 (8) | 0.075 (11) | 0.035 (7) | 0.014 (7) | 0.006 (6) | −0.015 (7) |
O19 | 0.055 (7) | 0.062 (8) | 0.037 (6) | 0.022 (6) | 0.026 (5) | −0.001 (5) |
C23 | 0.049 (5) | 0.061 (5) | 0.036 (4) | 0.016 (4) | 0.011 (4) | 0.006 (4) |
S2* | 0.0395 (18) | 0.045 (2) | 0.0320 (18) | 0.0090 (14) | 0.0111 (14) | −0.0046 (14) |
F4* | 0.077 (7) | 0.079 (8) | 0.069 (7) | −0.027 (6) | 0.034 (6) | 0.003 (6) |
F5* | 0.056 (3) | 0.084 (4) | 0.037 (2) | 0.015 (3) | 0.018 (2) | −0.010 (2) |
F6* | 0.057 (3) | 0.068 (3) | 0.065 (3) | 0.033 (3) | 0.020 (3) | 0.005 (3) |
O17* | 0.058 (7) | 0.064 (8) | 0.079 (9) | −0.006 (6) | 0.043 (7) | −0.018 (7) |
O18* | 0.053 (7) | 0.059 (8) | 0.027 (5) | 0.017 (6) | 0.013 (5) | −0.001 (5) |
O19* | 0.039 (5) | 0.040 (5) | 0.043 (5) | 0.010 (4) | 0.013 (4) | −0.008 (4) |
C23* | 0.049 (5) | 0.061 (5) | 0.036 (4) | 0.016 (4) | 0.011 (4) | 0.006 (4) |
O1W | 0.040 (3) | 0.034 (3) | 0.036 (3) | 0.012 (2) | 0.013 (2) | 0.002 (2) |
O2W | 0.041 (3) | 0.059 (3) | 0.035 (3) | 0.019 (3) | 0.012 (2) | −0.005 (2) |
Geometric parameters (Å, º) top
Nd1—O9 | 2.414 (4) | C5—H5A | 0.9500 |
Nd1—O9i | 2.436 (4) | C6—C9 | 1.424 (9) |
Nd1—O8 | 2.448 (4) | C6—C7 | 1.448 (8) |
Nd1—O6 | 2.467 (4) | C8—H8A | 0.9800 |
Nd1—O12 | 2.493 (4) | C8—H8B | 0.9800 |
Nd1—O1 | 2.494 (4) | C8—H8C | 0.9800 |
Nd1—O2 | 2.536 (4) | C9—H9A | 0.9500 |
Nd1—O7 | 2.549 (4) | C10—C11 | 1.445 (9) |
Nd1—O13 | 2.562 (5) | C10—H10A | 0.9500 |
Nd1—Nd2 | 3.7270 (4) | C11—C12 | 1.392 (9) |
Nd1—Nd1i | 3.7389 (6) | C11—C14 | 1.448 (7) |
Nd1—Nd2i | 4.1022 (4) | C12—C13 | 1.397 (9) |
Nd2—O9 | 2.425 (4) | C12—H12A | 0.9500 |
Nd2—O8 | 2.428 (4) | C13—C12i | 1.397 (9) |
Nd2—O8i | 2.435 (4) | C13—C15 | 1.513 (13) |
Nd2—O4 | 2.464 (4) | C14—C11i | 1.448 (7) |
Nd2—O3 | 2.470 (4) | C15—H15A | 0.9800 |
Nd2—O10 | 2.480 (4) | C15—H15B | 0.9800 |
Nd2—O11 | 2.554 (5) | C15—H15C | 0.9800 |
Nd2—O5 | 2.591 (4) | C16—C17 | 1.454 (10) |
Nd2—O2 | 2.596 (4) | C16—H16A | 0.9500 |
Nd2—Nd2i | 3.7436 (6) | C17—C18 | 1.407 (9) |
Nd2—Nd1i | 4.1022 (4) | C17—C20 | 1.424 (8) |
O1—C1 | 1.234 (7) | C18—C19 | 1.367 (10) |
O2—C7 | 1.292 (7) | C18—H18A | 0.9500 |
O3—C9 | 1.242 (8) | C19—C18i | 1.367 (10) |
O4—C10 | 1.233 (8) | C19—C21 | 1.526 (15) |
O5—C14 | 1.293 (10) | C20—C17i | 1.424 (8) |
O5—Nd2i | 2.591 (4) | C21—H21A | 0.9800 |
O6—C16 | 1.231 (8) | C21—H21B | 0.9800 |
O7—C20 | 1.294 (10) | C21—H21C | 0.9800 |
O7—Nd1i | 2.549 (4) | S1—O14 | 1.428 (5) |
O8—Nd2i | 2.435 (4) | S1—O16 | 1.435 (5) |
O8—H8O | 0.83 (5) | S1—O15 | 1.440 (5) |
O9—Nd1i | 2.436 (4) | S1—C22 | 1.784 (8) |
O9—H9O | 0.83 (5) | F1—C22 | 1.369 (11) |
O10—H10D | 0.8400 | F2—C22 | 1.299 (10) |
O10—H10E | 0.8399 | F3—C22 | 1.312 (10) |
O11—H11D | 0.8400 | S2—O19 | 1.426 (10) |
O11—H11E | 0.8401 | S2—O17 | 1.434 (12) |
O12—H12D | 0.8399 | S2—O18 | 1.435 (10) |
O12—H12E | 0.8400 | S2—C23 | 1.771 (8) |
O13—H13D | 0.8400 | F4—C23 | 1.445 (11) |
O13—H13E | 0.8398 | F5—C23 | 1.275 (8) |
C1—C2 | 1.439 (9) | F6—C23 | 1.306 (8) |
C1—H1A | 0.9500 | S2*—O19* | 1.421 (8) |
C2—C3 | 1.391 (9) | S2*—O17* | 1.437 (10) |
C2—C7 | 1.432 (9) | S2*—O18* | 1.442 (9) |
C3—C4 | 1.381 (11) | O1W—H1WA | 0.8402 |
C3—H3A | 0.9500 | O1W—H1WB | 0.8399 |
C4—C5 | 1.391 (12) | O2W—H2WA | 0.8400 |
C4—C8 | 1.531 (11) | O2W—H2WB | 0.8400 |
C5—C6 | 1.400 (9) | | |
| | | |
O9—Nd1—O9i | 73.58 (15) | Nd1—O2—Nd2 | 93.13 (13) |
O9—Nd1—O8 | 74.10 (13) | C9—O3—Nd2 | 136.9 (4) |
O9i—Nd1—O8 | 65.07 (13) | C10—O4—Nd2 | 137.3 (4) |
O9—Nd1—O6 | 133.07 (14) | C14—O5—Nd2 | 133.73 (9) |
O9i—Nd1—O6 | 92.30 (14) | C14—O5—Nd2i | 133.73 (9) |
O8—Nd1—O6 | 140.00 (13) | Nd2—O5—Nd2i | 92.53 (18) |
O9—Nd1—O12 | 90.07 (14) | C16—O6—Nd1 | 136.6 (4) |
O9i—Nd1—O12 | 141.03 (15) | C20—O7—Nd1 | 132.83 (9) |
O8—Nd1—O12 | 144.49 (14) | C20—O7—Nd1i | 132.83 (9) |
O6—Nd1—O12 | 73.17 (15) | Nd1—O7—Nd1i | 94.35 (19) |
O9—Nd1—O1 | 133.64 (13) | Nd2—O8—Nd2i | 100.69 (15) |
O9i—Nd1—O1 | 142.38 (14) | Nd2—O8—Nd1 | 99.69 (14) |
O8—Nd1—O1 | 94.75 (14) | Nd2i—O8—Nd1 | 114.30 (15) |
O6—Nd1—O1 | 83.75 (14) | Nd2—O8—H8O | 111 (5) |
O12—Nd1—O1 | 73.23 (16) | Nd2i—O8—H8O | 118 (5) |
O9—Nd1—O2 | 65.56 (13) | Nd1—O8—H8O | 111 (5) |
O9i—Nd1—O2 | 123.45 (13) | Nd1—O9—Nd2 | 100.74 (14) |
O8—Nd1—O2 | 67.26 (13) | Nd1—O9—Nd1i | 100.87 (14) |
O6—Nd1—O2 | 144.24 (14) | Nd2—O9—Nd1i | 115.08 (15) |
O12—Nd1—O2 | 77.28 (15) | Nd1—O9—H9O | 102 (5) |
O1—Nd1—O2 | 68.63 (13) | Nd2—O9—H9O | 117 (5) |
O9—Nd1—O7 | 65.45 (12) | Nd1i—O9—H9O | 116 (5) |
O9i—Nd1—O7 | 65.14 (12) | Nd2—O10—H10D | 102.8 |
O8—Nd1—O7 | 122.28 (13) | Nd2—O10—H10E | 119.2 |
O6—Nd1—O7 | 68.00 (13) | H10D—O10—H10E | 137.6 |
O12—Nd1—O7 | 75.90 (13) | Nd2—O11—H11D | 125.3 |
O1—Nd1—O7 | 142.97 (15) | Nd2—O11—H11E | 110.4 |
O2—Nd1—O7 | 123.24 (10) | H11D—O11—H11E | 118.5 |
O9—Nd1—O13 | 145.25 (14) | Nd1—O12—H12D | 122.7 |
O9i—Nd1—O13 | 77.86 (14) | Nd1—O12—H12E | 123.6 |
O8—Nd1—O13 | 76.16 (15) | H12D—O12—H12E | 113.6 |
O6—Nd1—O13 | 66.67 (16) | Nd1—O13—H13D | 107.1 |
O12—Nd1—O13 | 124.69 (15) | Nd1—O13—H13E | 120.7 |
O1—Nd1—O13 | 66.21 (15) | H13D—O13—H13E | 102.1 |
O2—Nd1—O13 | 117.72 (16) | O1—C1—C2 | 127.9 (6) |
O7—Nd1—O13 | 118.76 (12) | O1—C1—H1A | 116.1 |
O9—Nd1—Nd2 | 39.74 (9) | C2—C1—H1A | 116.1 |
O9i—Nd1—Nd2 | 79.57 (9) | C3—C2—C7 | 120.8 (6) |
O8—Nd1—Nd2 | 39.95 (9) | C3—C2—C1 | 115.9 (6) |
O6—Nd1—Nd2 | 170.44 (10) | C7—C2—C1 | 123.2 (5) |
O12—Nd1—Nd2 | 110.15 (11) | C4—C3—C2 | 123.8 (7) |
O1—Nd1—Nd2 | 105.75 (10) | C4—C3—H3A | 118.1 |
O2—Nd1—Nd2 | 44.07 (9) | C2—C3—H3A | 118.1 |
O7—Nd1—Nd2 | 103.70 (8) | C3—C4—C5 | 116.3 (7) |
O13—Nd1—Nd2 | 115.82 (12) | C3—C4—C8 | 121.2 (8) |
O9—Nd1—Nd1i | 39.79 (9) | C5—C4—C8 | 122.4 (8) |
O9i—Nd1—Nd1i | 39.34 (9) | C4—C5—C6 | 122.9 (7) |
O8—Nd1—Nd1i | 79.82 (9) | C4—C5—H5A | 118.5 |
O6—Nd1—Nd1i | 103.85 (10) | C6—C5—H5A | 118.5 |
O12—Nd1—Nd1i | 108.17 (11) | C5—C6—C9 | 115.7 (6) |
O1—Nd1—Nd1i | 172.38 (10) | C5—C6—C7 | 120.6 (6) |
O2—Nd1—Nd1i | 104.16 (9) | C9—C6—C7 | 123.7 (5) |
O7—Nd1—Nd1i | 42.83 (9) | O2—C7—C2 | 122.7 (5) |
O13—Nd1—Nd1i | 117.03 (11) | O2—C7—C6 | 122.0 (5) |
Nd2—Nd1—Nd1i | 66.660 (7) | C2—C7—C6 | 115.3 (5) |
O9—Nd1—Nd2i | 72.01 (9) | C4—C8—H8A | 109.5 |
O9i—Nd1—Nd2i | 32.38 (9) | C4—C8—H8B | 109.5 |
O8—Nd1—Nd2i | 32.74 (9) | H8A—C8—H8B | 109.5 |
O6—Nd1—Nd2i | 117.60 (10) | C4—C8—H8C | 109.5 |
O12—Nd1—Nd2i | 161.97 (11) | H8A—C8—H8C | 109.5 |
O1—Nd1—Nd2i | 120.58 (11) | H8B—C8—H8C | 109.5 |
O2—Nd1—Nd2i | 96.38 (9) | O3—C9—C6 | 127.0 (5) |
O7—Nd1—Nd2i | 94.28 (8) | O3—C9—H9A | 116.5 |
O13—Nd1—Nd2i | 73.26 (10) | C6—C9—H9A | 116.5 |
Nd2—Nd1—Nd2i | 56.888 (9) | O4—C10—C11 | 127.5 (6) |
Nd1i—Nd1—Nd2i | 56.531 (7) | O4—C10—H10A | 116.2 |
O9—Nd2—O8 | 74.27 (13) | C11—C10—H10A | 116.2 |
O9—Nd2—O8i | 65.45 (13) | C12—C11—C10 | 115.8 (6) |
O8—Nd2—O8i | 74.31 (15) | C12—C11—C14 | 121.0 (6) |
O9—Nd2—O4 | 145.49 (14) | C10—C11—C14 | 123.2 (6) |
O8—Nd2—O4 | 132.36 (14) | C11—C12—C13 | 123.6 (7) |
O8i—Nd2—O4 | 97.66 (14) | C11—C12—H12A | 118.2 |
O9—Nd2—O3 | 94.83 (14) | C13—C12—H12A | 118.2 |
O8—Nd2—O3 | 133.19 (13) | C12i—C13—C12 | 115.8 (8) |
O8i—Nd2—O3 | 142.48 (14) | C12i—C13—C15 | 122.1 (4) |
O4—Nd2—O3 | 80.76 (14) | C12—C13—C15 | 122.1 (4) |
O9—Nd2—O10 | 138.36 (14) | O5—C14—C11i | 122.5 (4) |
O8—Nd2—O10 | 84.30 (14) | O5—C14—C11 | 122.5 (4) |
O8i—Nd2—O10 | 141.55 (14) | C11i—C14—C11 | 114.9 (7) |
O4—Nd2—O10 | 73.63 (16) | C13—C15—H15A | 109.5 |
O3—Nd2—O10 | 74.34 (15) | C13—C15—H15B | 109.5 |
O9—Nd2—O11 | 78.62 (14) | H15A—C15—H15B | 109.5 |
O8—Nd2—O11 | 147.38 (14) | C13—C15—H15C | 109.5 |
O8i—Nd2—O11 | 78.16 (14) | H15A—C15—H15C | 109.5 |
O4—Nd2—O11 | 68.20 (16) | H15B—C15—H15C | 109.5 |
O3—Nd2—O11 | 66.38 (15) | O6—C16—C17 | 127.0 (6) |
O10—Nd2—O11 | 128.31 (14) | O6—C16—H16A | 116.5 |
O9—Nd2—O5 | 122.73 (13) | C17—C16—H16A | 116.5 |
O8—Nd2—O5 | 65.60 (11) | C18—C17—C20 | 121.3 (7) |
O8i—Nd2—O5 | 65.51 (12) | C18—C17—C16 | 116.1 (6) |
O4—Nd2—O5 | 68.43 (13) | C20—C17—C16 | 122.7 (6) |
O3—Nd2—O5 | 142.44 (14) | C19—C18—C17 | 122.1 (7) |
O10—Nd2—O5 | 76.69 (12) | C19—C18—H18A | 119.0 |
O11—Nd2—O5 | 117.42 (13) | C17—C18—H18A | 119.0 |
O9—Nd2—O2 | 64.46 (13) | C18—C19—C18i | 118.0 (10) |
O8—Nd2—O2 | 66.59 (12) | C18—C19—C21 | 121.0 (5) |
O8i—Nd2—O2 | 122.49 (13) | C18i—C19—C21 | 121.0 (5) |
O4—Nd2—O2 | 139.86 (14) | O7—C20—C17i | 122.5 (4) |
O3—Nd2—O2 | 67.70 (13) | O7—C20—C17 | 122.5 (4) |
O10—Nd2—O2 | 74.37 (14) | C17i—C20—C17 | 115.0 (8) |
O11—Nd2—O2 | 116.69 (16) | C19—C21—H21A | 109.5 |
O5—Nd2—O2 | 125.65 (9) | C19—C21—H21B | 109.5 |
O9—Nd2—Nd1 | 39.51 (9) | H21A—C21—H21B | 109.5 |
O8—Nd2—Nd1 | 40.36 (9) | C19—C21—H21C | 109.5 |
O8i—Nd2—Nd1 | 80.22 (9) | H21A—C21—H21C | 109.5 |
O4—Nd2—Nd1 | 172.71 (10) | H21B—C21—H21C | 109.5 |
O3—Nd2—Nd1 | 105.21 (10) | O14—S1—O16 | 114.4 (4) |
O10—Nd2—Nd1 | 103.65 (11) | O14—S1—O15 | 115.1 (4) |
O11—Nd2—Nd1 | 117.82 (11) | O16—S1—O15 | 114.5 (3) |
O5—Nd2—Nd1 | 104.45 (8) | O14—S1—C22 | 102.2 (4) |
O2—Nd2—Nd1 | 42.80 (9) | O16—S1—C22 | 103.6 (4) |
O9—Nd2—Nd2i | 79.34 (9) | O15—S1—C22 | 104.9 (4) |
O8—Nd2—Nd2i | 39.72 (9) | F2—C22—F3 | 110.7 (8) |
O8i—Nd2—Nd2i | 39.59 (9) | F2—C22—F1 | 104.6 (9) |
O4—Nd2—Nd2i | 107.33 (10) | F3—C22—F1 | 103.8 (9) |
O3—Nd2—Nd2i | 171.78 (10) | F2—C22—S1 | 113.7 (7) |
O10—Nd2—Nd2i | 106.14 (10) | F3—C22—S1 | 113.7 (7) |
O11—Nd2—Nd2i | 117.50 (11) | F1—C22—S1 | 109.4 (7) |
O5—Nd2—Nd2i | 43.73 (9) | O19—S2—O17 | 112.8 (9) |
O2—Nd2—Nd2i | 104.36 (9) | O19—S2—O18 | 116.4 (8) |
Nd1—Nd2—Nd2i | 66.612 (7) | O17—S2—O18 | 115.1 (10) |
O9—Nd2—Nd1i | 32.54 (9) | O19—S2—C23 | 105.4 (5) |
O8—Nd2—Nd1i | 72.51 (9) | O17—S2—C23 | 98.6 (7) |
O8i—Nd2—Nd1i | 32.95 (9) | O18—S2—C23 | 106.1 (7) |
O4—Nd2—Nd1i | 124.01 (11) | F5—C23—F6 | 113.4 (7) |
O3—Nd2—Nd1i | 120.44 (10) | F5—C23—F4 | 95.3 (7) |
O10—Nd2—Nd1i | 156.72 (10) | F6—C23—F4 | 100.1 (8) |
O11—Nd2—Nd1i | 74.87 (10) | F5—C23—S2 | 120.7 (5) |
O5—Nd2—Nd1i | 95.08 (8) | F6—C23—S2 | 114.9 (6) |
O2—Nd2—Nd1i | 93.99 (9) | F4—C23—S2 | 107.8 (7) |
Nd1—Nd2—Nd1i | 56.809 (9) | O19*—S2*—O17* | 115.7 (7) |
Nd2i—Nd2—Nd1i | 56.499 (7) | O19*—S2*—O18* | 113.7 (7) |
C1—O1—Nd1 | 135.6 (4) | O17*—S2*—O18* | 115.7 (8) |
C7—O2—Nd1 | 134.8 (4) | H1WA—O1W—H1WB | 121.4 |
C7—O2—Nd2 | 131.8 (4) | H2WA—O2W—H2WB | 128.4 |
Symmetry code: (i) −x+1, y, −z+1/2. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O8—H8O···O18 | 0.83 (5) | 2.10 (6) | 2.891 (13) | 158 (7) |
O9—H9O···O15 | 0.83 (5) | 2.19 (6) | 2.982 (6) | 159 (6) |
O10—H10D···O18 | 0.84 | 1.89 | 2.729 (11) | 180 |
O10—H10E···O1Wii | 0.84 | 1.98 | 2.816 (6) | 180 |
O11—H11D···O1W | 0.84 | 2.10 | 2.937 (7) | 179 |
O11—H11E···O19i | 0.84 | 2.12 | 2.955 (11) | 180 |
O12—H12D···O16 | 0.84 | 1.95 | 2.794 (7) | 180 |
O12—H12E···O2Wiii | 0.84 | 1.97 | 2.806 (7) | 180 |
O13—H13D···O11i | 0.84 | 1.86 | 2.698 (7) | 180 |
O13—H13E···O2Wi | 0.84 | 2.02 | 2.862 (8) | 180 |
O1W—H1WA···O14 | 0.84 | 2.01 | 2.850 (8) | 180 |
O1W—H1WB···C9ii | 0.84 | 2.33 | 3.167 (8) | 180 |
O2W—H2WA···O15 | 0.84 | 2.19 | 3.034 (8) | 180 |
O2W—H2WB···C16iv | 0.84 | 2.44 | 3.276 (8) | 180 |
Symmetry codes: (i) −x+1, y, −z+1/2; (ii) −x+1/2, −y+1/2, −z; (iii) x, −y, z+1/2; (iv) x, −y, z−1/2. |
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