catena-Poly[[[diaqua­neodymium(III)]bis­(μ-difluoro­acetato-κ2O:O′)[diaqua­neodymium(III)]tetra­kis(μ-difluoro­acetato-κ2O:O′)] monohydrate]

Rohde, A.; Urland, W.

doi:10.1107/S1600536806045910

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catena-Poly[[[diaquaneodymium(III)]bis(μ-difluoroacetato-κ²O:O′)[diaquaneodymium(III)]tetrakis(μ-difluoroacetato-κ²O:O′)] monohydrate]

A. Rohde and W. Urland

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.

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Supporting information

	Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806045910/sg2083sup1.cif Contains datablocks global, I
	Structure factor file (CIF format) https://doi.org/10.1107/S1600536806045910/sg2083Isup2.hkl Contains datablock I

CCDC reference: 630455

checkCIF report

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

Computing details top

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
M_r = 483.37	F(000) = 462
Triclinic, P1	D_x = 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	R_int = 0.042
Graphite monochromator	θ_max = 26.1°, θ_min = 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(F_o²) + (0.0443P)²] where P = (F_o² + 2F_c²)/3
2512 reflections	(Δ/σ)_max = 0.001
199 parameters	Δρ_max = 0.69 e Å⁻³
0 restraints	Δρ_min = −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	U_iso*/U_eq
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···F11^iv	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···F32^v	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.

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