The title compound, {[Nd(C2HF2O2)3(H2O)2]·H2O}n, was synthesized by the reaction of Nd2O3 with difluoroacetic acid in water. The compound consists of chains, running along the b axis. The Nd3+ ion is coordinated by eight O atoms, giving a distorted square antiprism.
Supporting information
CCDC reference: 630455
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (C-C) = 0.007 Å
- R factor = 0.026
- wR factor = 0.064
- Data-to-parameter ratio = 12.6
checkCIF/PLATON results
No syntax errors found
Alert level B
PLAT029_ALERT_3_B _diffrn_measured_fraction_theta_full Low ....... 0.94
PLAT242_ALERT_2_B Check Low Ueq as Compared to Neighbors for C12
Alert level C
PLAT022_ALERT_3_C Ratio Unique / Expected Reflections too Low .... 0.92
PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for Nd1
PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C22
PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C32
PLAT764_ALERT_4_C Overcomplete CIF Bond List Detected (Rep/Expd) . 1.13 Ratio
Alert level G
PLAT199_ALERT_1_G Check the Reported _cell_measurement_temperature 293 K
0 ALERT level A = In general: serious problem
2 ALERT level B = Potentially serious problem
5 ALERT level C = Check and explain
1 ALERT level G = General alerts; check
1 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
4 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
1 ALERT type 4 Improvement, methodology, query or suggestion
0 ALERT type 5 Informative message, check
Data collection: IPDS Software (Stoe & Cie, 1998); cell refinement: IPDS Software; data reduction: IPDS Software; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: DIAMOND (Brandenburg, 2006); software used to prepare material for publication: SHELXL97.
catena-Poly[[diaquaneodymium(III)]bis(µ-difluoroacetato-
κ2O:
O')[diaquaneodymium(III)]tetrakis(µ-difluoroacetato-
κ2O:
O')] monohydrate]
top
Crystal data top
[Nd(C2HF2O2)3(H2O)2]·H2O | Z = 2 |
Mr = 483.37 | F(000) = 462 |
Triclinic, P1 | Dx = 2.337 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71073 Å |
a = 8.405 (2) Å | Cell parameters from 8000 reflections |
b = 9.508 (3) Å | θ = 2.5–25.8° |
c = 9.639 (3) Å | µ = 3.90 mm−1 |
α = 66.67 (3)° | T = 293 K |
β = 79.34 (3)° | Block, violet |
γ = 77.74 (3)° | 0.22 × 0.13 × 0.13 mm |
V = 686.8 (4) Å3 | |
Data collection top
Stoe IPDS area-detector diffractometer | 2246 reflections with I > 2σ(I) |
Radiation source: fine-focus sealed tube | Rint = 0.042 |
Graphite monochromator | θmax = 26.1°, θmin = 2.3° |
φ scans | h = −10→10 |
9819 measured reflections | k = −11→11 |
2512 independent reflections | l = −11→11 |
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)] = 0.026 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.064 | H-atom parameters constrained |
S = 1.04 | w = 1/[σ2(Fo2) + (0.0443P)2] where P = (Fo2 + 2Fc2)/3 |
2512 reflections | (Δ/σ)max = 0.001 |
199 parameters | Δρmax = 0.69 e Å−3 |
0 restraints | Δρmin = −1.20 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 | |
Nd1 | 0.51780 (3) | 0.74338 (3) | 0.95909 (2) | 0.01926 (9) | |
O11 | 0.6703 (4) | 0.6931 (4) | 0.7303 (4) | 0.0338 (8) | |
O12 | 0.6063 (5) | 0.4555 (5) | 0.8373 (4) | 0.0453 (10) | |
C11 | 0.6718 (5) | 0.5620 (6) | 0.7318 (5) | 0.0246 (10) | |
C12 | 0.7621 (6) | 0.5203 (7) | 0.5972 (6) | 0.0369 (12) | |
H12 | 0.8534 | 0.4361 | 0.6312 | 0.044* | |
F11 | 0.6611 (6) | 0.4764 (8) | 0.5379 (6) | 0.104 (2) | |
F12 | 0.8193 (6) | 0.6438 (6) | 0.4865 (4) | 0.0785 (13) | |
O21 | 0.2891 (4) | 0.7144 (4) | 0.8503 (4) | 0.0330 (8) | |
O22 | 0.2598 (4) | 0.4619 (4) | 0.9458 (4) | 0.0340 (8) | |
C21 | 0.2207 (5) | 0.6023 (6) | 0.8685 (5) | 0.0247 (9) | |
C22 | 0.0638 (5) | 0.6408 (6) | 0.7932 (5) | 0.0300 (10) | |
H22 | −0.0294 | 0.6662 | 0.8616 | 0.036* | |
F21 | 0.0702 (5) | 0.7618 (5) | 0.6603 (4) | 0.0686 (13) | |
F22 | 0.0404 (5) | 0.5198 (5) | 0.7663 (6) | 0.0775 (14) | |
O31 | 0.7440 (4) | 0.8944 (4) | 0.8720 (4) | 0.0339 (8) | |
O32 | 0.6904 (4) | 1.0784 (5) | 0.9692 (4) | 0.0434 (9) | |
C31 | 0.7767 (5) | 1.0047 (6) | 0.8929 (5) | 0.0243 (9) | |
C32 | 0.9437 (6) | 1.0530 (7) | 0.8145 (6) | 0.0335 (11) | |
H32 | 1.0298 | 0.9622 | 0.8381 | 0.040* | |
F31 | 0.9805 (5) | 1.1619 (5) | 0.8542 (5) | 0.0607 (10) | |
F32 | 0.9336 (5) | 1.1173 (5) | 0.6630 (4) | 0.0677 (12) | |
O1W | 0.4591 (4) | 0.9871 (4) | 0.7197 (3) | 0.0317 (7) | |
H11W | 0.5622 | 0.9676 | 0.6986 | 0.038* | |
H12W | 0.4157 | 0.9227 | 0.7037 | 0.038* | |
O2W | 0.5945 (5) | 0.7552 (5) | 1.1921 (4) | 0.0465 (10) | |
H21W | 0.6095 | 0.6844 | 1.2786 | 0.056* | |
H22W | 0.6328 | 0.8332 | 1.1869 | 0.056* | |
O3W | 0.2727 (5) | 1.0115 (5) | 0.5003 (4) | 0.0440 (9) | |
H31W | 0.1694 | 1.0167 | 0.5078 | 0.053* | |
H32W | 0.2922 | 1.0997 | 0.4894 | 0.053* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Nd1 | 0.01826 (12) | 0.01679 (15) | 0.02294 (12) | −0.00531 (8) | −0.00079 (7) | −0.00696 (9) |
O11 | 0.0430 (19) | 0.026 (2) | 0.0324 (17) | −0.0034 (15) | −0.0008 (14) | −0.0139 (14) |
O12 | 0.050 (2) | 0.048 (3) | 0.0329 (18) | −0.0334 (19) | −0.0021 (15) | 0.0024 (16) |
C11 | 0.0204 (19) | 0.027 (3) | 0.026 (2) | −0.0061 (17) | −0.0033 (16) | −0.0080 (18) |
C12 | 0.038 (3) | 0.043 (4) | 0.038 (3) | −0.012 (2) | 0.003 (2) | −0.023 (2) |
F11 | 0.082 (3) | 0.193 (7) | 0.099 (4) | −0.059 (4) | 0.012 (3) | −0.110 (4) |
F12 | 0.112 (3) | 0.069 (3) | 0.044 (2) | −0.033 (3) | 0.035 (2) | −0.0191 (19) |
O21 | 0.0280 (16) | 0.029 (2) | 0.0440 (19) | −0.0098 (14) | −0.0116 (13) | −0.0095 (15) |
O22 | 0.0330 (17) | 0.020 (2) | 0.0461 (19) | 0.0016 (13) | −0.0130 (14) | −0.0079 (15) |
C21 | 0.0202 (19) | 0.027 (3) | 0.029 (2) | −0.0036 (17) | 0.0005 (16) | −0.0130 (19) |
C22 | 0.025 (2) | 0.025 (3) | 0.039 (2) | −0.0063 (18) | −0.0088 (18) | −0.007 (2) |
F21 | 0.061 (2) | 0.077 (3) | 0.051 (2) | −0.031 (2) | −0.0305 (17) | 0.0151 (18) |
F22 | 0.071 (3) | 0.051 (3) | 0.139 (4) | 0.0035 (19) | −0.064 (3) | −0.049 (3) |
O31 | 0.0309 (17) | 0.035 (2) | 0.0435 (19) | −0.0178 (15) | −0.0001 (14) | −0.0177 (16) |
O32 | 0.0384 (19) | 0.038 (3) | 0.051 (2) | 0.0011 (16) | 0.0126 (16) | −0.0244 (18) |
C31 | 0.0153 (18) | 0.028 (3) | 0.027 (2) | −0.0019 (16) | −0.0014 (15) | −0.0093 (18) |
C32 | 0.028 (2) | 0.036 (3) | 0.042 (3) | −0.017 (2) | 0.0025 (19) | −0.017 (2) |
F31 | 0.062 (2) | 0.054 (3) | 0.084 (3) | −0.0344 (19) | −0.0049 (19) | −0.032 (2) |
F32 | 0.071 (2) | 0.091 (3) | 0.0381 (18) | −0.045 (2) | 0.0112 (16) | −0.0123 (18) |
O1W | 0.0378 (17) | 0.028 (2) | 0.0293 (16) | −0.0058 (14) | −0.0051 (13) | −0.0102 (14) |
O2W | 0.082 (3) | 0.028 (2) | 0.0360 (19) | −0.0135 (19) | −0.0196 (18) | −0.0101 (16) |
O3W | 0.040 (2) | 0.044 (3) | 0.043 (2) | −0.0131 (17) | −0.0056 (16) | −0.0077 (17) |
Geometric parameters (Å, º) top
Nd1—O32i | 2.374 (4) | O22—Nd1ii | 2.411 (3) |
Nd1—O12ii | 2.378 (3) | C21—C22 | 1.529 (6) |
Nd1—O22ii | 2.411 (3) | C22—F22 | 1.334 (6) |
Nd1—O31 | 2.448 (3) | C22—F21 | 1.342 (6) |
Nd1—O21 | 2.464 (3) | C22—H22 | 0.9800 |
Nd1—O2W | 2.497 (4) | O31—C31 | 1.236 (6) |
Nd1—O11 | 2.502 (3) | O32—C31 | 1.246 (6) |
Nd1—O1W | 2.577 (3) | O32—Nd1i | 2.374 (4) |
Nd1—H11W | 2.5960 | C31—C32 | 1.536 (6) |
Nd1—H12W | 2.5576 | C32—F31 | 1.345 (6) |
O11—C11 | 1.238 (6) | C32—F32 | 1.353 (6) |
O12—C11 | 1.256 (6) | C32—H32 | 0.9800 |
O12—Nd1ii | 2.378 (3) | O1W—H11W | 0.8499 |
C11—C12 | 1.527 (6) | O1W—H12W | 0.8500 |
C12—F11 | 1.319 (6) | O2W—H21W | 0.8500 |
C12—F12 | 1.344 (7) | O2W—H22W | 0.8500 |
C12—H12 | 0.9800 | O3W—H31W | 0.8500 |
O21—C21 | 1.254 (6) | O3W—H32W | 0.8501 |
O22—C21 | 1.250 (6) | | |
| | | |
O32i—Nd1—O12ii | 86.60 (15) | O1W—Nd1—H12W | 19.1 |
O32i—Nd1—O22ii | 142.27 (13) | H11W—Nd1—H12W | 30.9 |
O12ii—Nd1—O22ii | 74.62 (14) | C11—O11—Nd1 | 115.3 (3) |
O32i—Nd1—O31 | 99.69 (13) | C11—O12—Nd1ii | 178.7 (4) |
O12ii—Nd1—O31 | 146.06 (12) | O11—C11—O12 | 125.6 (4) |
O22ii—Nd1—O31 | 80.60 (13) | O11—C11—C12 | 119.2 (4) |
O32i—Nd1—O21 | 81.16 (13) | O12—C11—C12 | 115.2 (5) |
O12ii—Nd1—O21 | 76.42 (12) | F11—C12—F12 | 106.9 (5) |
O22ii—Nd1—O21 | 123.83 (12) | F11—C12—C11 | 110.2 (4) |
O31—Nd1—O21 | 137.40 (12) | F12—C12—C11 | 110.9 (4) |
O32i—Nd1—O2W | 73.36 (14) | F11—C12—H12 | 109.6 |
O12ii—Nd1—O2W | 75.91 (13) | F12—C12—H12 | 109.6 |
O22ii—Nd1—O2W | 70.49 (13) | C11—C12—H12 | 109.6 |
O31—Nd1—O2W | 74.14 (13) | C21—O21—Nd1 | 134.2 (3) |
O21—Nd1—O2W | 143.14 (13) | C21—O22—Nd1ii | 145.8 (3) |
O32i—Nd1—O11 | 141.86 (13) | O22—C21—O21 | 128.6 (4) |
O12ii—Nd1—O11 | 120.25 (14) | O22—C21—C22 | 114.7 (4) |
O22ii—Nd1—O11 | 74.88 (12) | O21—C21—C22 | 116.7 (4) |
O31—Nd1—O11 | 73.60 (12) | F22—C22—F21 | 108.0 (4) |
O21—Nd1—O11 | 79.96 (12) | F22—C22—C21 | 110.6 (4) |
O2W—Nd1—O11 | 135.64 (13) | F21—C22—C21 | 111.4 (4) |
O32i—Nd1—O1W | 71.63 (13) | F22—C22—H22 | 108.9 |
O12ii—Nd1—O1W | 143.35 (12) | F21—C22—H22 | 108.9 |
O22ii—Nd1—O1W | 139.08 (12) | C21—C22—H22 | 108.9 |
O31—Nd1—O1W | 68.66 (12) | C31—O31—Nd1 | 135.6 (3) |
O21—Nd1—O1W | 71.45 (12) | C31—O32—Nd1i | 161.1 (4) |
O2W—Nd1—O1W | 122.49 (12) | O31—C31—O32 | 127.4 (4) |
O11—Nd1—O1W | 71.03 (12) | O31—C31—C32 | 114.6 (4) |
O32i—Nd1—H11W | 87.0 | O32—C31—C32 | 118.0 (4) |
O12ii—Nd1—H11W | 160.3 | F31—C32—F32 | 106.8 (4) |
O22ii—Nd1—H11W | 120.4 | F31—C32—C31 | 112.0 (4) |
O31—Nd1—H11W | 53.6 | F32—C32—C31 | 107.5 (4) |
O21—Nd1—H11W | 84.2 | F31—C32—H32 | 110.1 |
O2W—Nd1—H11W | 119.8 | F32—C32—H32 | 110.1 |
O11—Nd1—H11W | 58.4 | C31—C32—H32 | 110.1 |
O1W—Nd1—H11W | 18.9 | Nd1—O1W—H11W | 81.8 |
O32i—Nd1—H12W | 78.1 | Nd1—O1W—H12W | 79.2 |
O12ii—Nd1—H12W | 129.4 | H11W—O1W—H12W | 107.7 |
O22ii—Nd1—H12W | 138.7 | Nd1—O2W—H21W | 130.5 |
O31—Nd1—H12W | 84.4 | Nd1—O2W—H22W | 120.3 |
O21—Nd1—H12W | 53.8 | H21W—O2W—H22W | 107.7 |
O2W—Nd1—H12W | 140.4 | H31W—O3W—H32W | 107.7 |
O11—Nd1—H12W | 64.0 | | |
| | | |
O32i—Nd1—O11—C11 | −127.7 (3) | Nd1—O21—C21—O22 | −5.4 (7) |
O12ii—Nd1—O11—C11 | 1.4 (3) | Nd1—O21—C21—C22 | 171.3 (3) |
O22ii—Nd1—O11—C11 | 63.0 (3) | O22—C21—C22—F22 | −28.1 (6) |
O31—Nd1—O11—C11 | 147.5 (3) | O21—C21—C22—F22 | 154.7 (4) |
O21—Nd1—O11—C11 | −66.3 (3) | O22—C21—C22—F21 | −148.2 (5) |
O2W—Nd1—O11—C11 | 102.6 (3) | O21—C21—C22—F21 | 34.6 (6) |
O1W—Nd1—O11—C11 | −140.0 (3) | O32i—Nd1—O31—C31 | 20.9 (5) |
Nd1—O11—C11—O12 | −1.0 (6) | O12ii—Nd1—O31—C31 | −77.5 (5) |
Nd1—O11—C11—C12 | −179.9 (3) | O22ii—Nd1—O31—C31 | −120.8 (4) |
O11—C11—C12—F11 | −122.8 (6) | O21—Nd1—O31—C31 | 108.4 (4) |
O12—C11—C12—F11 | 58.1 (7) | O2W—Nd1—O31—C31 | −48.6 (4) |
O11—C11—C12—F12 | −4.7 (6) | O11—Nd1—O31—C31 | 162.3 (5) |
O12—C11—C12—F12 | 176.2 (5) | O1W—Nd1—O31—C31 | 86.7 (4) |
O32i—Nd1—O21—C21 | −121.9 (4) | Nd1—O31—C31—O32 | −2.5 (8) |
O12ii—Nd1—O21—C21 | −33.3 (4) | Nd1—O31—C31—C32 | 177.3 (3) |
O22ii—Nd1—O21—C21 | 27.3 (5) | Nd1i—O32—C31—O31 | −78.8 (13) |
O31—Nd1—O21—C21 | 143.3 (4) | Nd1i—O32—C31—C32 | 101.4 (10) |
O2W—Nd1—O21—C21 | −75.6 (5) | O31—C31—C32—F31 | −173.3 (4) |
O11—Nd1—O21—C21 | 91.4 (4) | O32—C31—C32—F31 | 6.5 (7) |
O1W—Nd1—O21—C21 | 164.6 (4) | O31—C31—C32—F32 | 69.7 (6) |
Nd1ii—O22—C21—O21 | −31.5 (9) | O32—C31—C32—F32 | −110.5 (5) |
Nd1ii—O22—C21—C22 | 151.7 (4) | | |
Symmetry codes: (i) −x+1, −y+2, −z+2; (ii) −x+1, −y+1, −z+2. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O1W—H11W···O3Wiii | 0.85 | 2.12 | 2.793 (5) | 136 |
O1W—H11W···O31 | 0.85 | 2.28 | 2.836 (5) | 124 |
O1W—H11W···O11 | 0.85 | 2.49 | 2.951 (5) | 115 |
O1W—H12W···O3W | 0.85 | 2.26 | 2.768 (5) | 118 |
O1W—H12W···O21 | 0.85 | 2.27 | 2.945 (5) | 136 |
O2W—H21W···F11iv | 0.85 | 2.54 | 3.393 (8) | 178 |
O2W—H22W···O1Wi | 0.85 | 2.17 | 2.823 (5) | 133 |
O2W—H22W···O32 | 0.85 | 2.51 | 3.145 (6) | 132 |
O3W—H31W···F32v | 0.85 | 2.51 | 3.157 (6) | 134 |
O3W—H31W···F21 | 0.85 | 2.51 | 2.959 (5) | 114 |
O3W—H32W···O11iii | 0.85 | 2.28 | 2.880 (6) | 128 |
Symmetry codes: (i) −x+1, −y+2, −z+2; (iii) −x+1, −y+2, −z+1; (iv) x, y, z+1; (v) x−1, y, z. |