Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536805011785/hb6176sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536805011785/hb6176Isup2.hkl |
CCDC reference: 271882
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.
[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 |
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 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 |
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. |
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* |
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) |
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. |
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. |