Ammonium neodymium(III) bis­[sulfate­(VI)] tetra­hydrate

(NH₄)[Nd(SO₄)₂(H₂O)₃]·H₂O is isotypic with other members of the (NH₄)[Ln(SO₄)₂(H₂O)₃]·H₂O family (Ln = lanthanides). It contains NdO₉ polyhedra and SO₄ tetra­hedra, which are linked by common edges and vertices, forming a layer-like arrangement parallel to (010). The neodymium cation is nine-coordinated in a distorted monocapped square anti­prismatic geometry with two sulfate groups as chelating and two sulfate groups as bridging ligands. O—H...O and N—H...O hydrogen bonds consolidate the structure into a three-dimensional network. The dependence of unit-cell dimensions of the isotypic compounds on the lanthanide atomic number is discussed.

Key indicators

• Single-crystal X-ray study
• T = 291 K
• Mean [sigma](S-O) = 0.003 Å
• R factor = 0.024
• wR factor = 0.058
• Data-to-parameter ratio = 22.1

checkCIF/PLATON results

No syntax errors found



Alert level C
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ ....          ?
PLAT220_ALERT_2_C Large Non-Solvent    O     Ueq(max)/Ueq(min) ...       2.63 Ratio
PLAT241_ALERT_2_C Check High      Ueq as Compared to Neighbors for        O21
PLAT241_ALERT_2_C Check High      Ueq as Compared to Neighbors for        O22
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         S2

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:   H12 N1 Nd1 O12 S2
            Atom count from _chemical_formula_moiety:H16 N2 Nd1 O12 S2

   0 ALERT level A = In general: serious problem
   0 ALERT level B = Potentially serious problem
   6 ALERT level C = Check and explain
   1 ALERT level G = General alerts; check

   2 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
   5 ALERT type 2 Indicator that the structure model may be wrong or deficient
   0 ALERT type 3 Indicator that the structure quality may be low
   0 ALERT type 4 Improvement, methodology, query or suggestion

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Computing details

Data collection: KM-4 Software (Kuma, 1993); cell refinement: KM-4 Software; data reduction: DATAPROC (Gałdecki et al., 1998); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: XP in SHELXTL (Sheldrick, 1990), ORTEP-3 (Farrugia, 1997) and Mercury (Bruno et al., 2002); software used to prepare material for publication: SHELXL97.

Ammonium neodymium(III) bis[sulfate(VI)] tetrahydrate

Crystal data

(NH4)[Nd(SO4)2(H2O)3].H2O	F(000) = 828
Mr = 426.47	Dx = 2.585 Mg m^−3
Monoclinic, P21/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybc	Cell parameters from 99 reflections
a = 6.636 (1) Å	θ = 5–25°
b = 18.935 (1) Å	µ = 5.18 mm^−1
c = 8.789 (1) Å	T = 291 K
β = 97.06 (1)°	Prism, light violet
V = 1096.0 (2) Å^3	0.06 × 0.04 × 0.03 mm
Z = 4

Data collection

Kuma KM-4 diffractometer	2939 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tube	Rint = 0.019
Graphite monochromator	θmax = 30.1°, θmin = 2.2°
ω/2θ scans	h = −9→9
Absorption correction: numerical (X-RED32; Stoe & Cie, 1999)	k = −1→26
Tmin = 0.764, Tmax = 0.869	l = −1→12
3999 measured reflections	3 standard reflections every 100 reflections
3224 independent reflections	intensity decay: 72.3%

Refinement

Refinement on F^2	Secondary atom site location: structure-invariant direct methods
Least-squares matrix: full	Hydrogen site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.025	H-atom parameters constrained
wR(F^2) = 0.058	w = 1/[σ^2(Fo^2) + (0.0232P)^2 + 3.8961P] where P = (Fo^2 + 2Fc^2)/3
S = 1.04	(Δ/σ)max < 0.001
3224 reflections	Δρmax = 1.58 e Å^−3
146 parameters	Δρmin = −1.02 e Å^−3
0 restraints	Extinction correction: SHELXL97, Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
Primary atom site location: structure-invariant direct methods	Extinction coefficient: 0.0150 (4)

Special details

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 (Ų)

	x	y	z	Uiso*/Ueq
Nd1	0.14675 (2)	0.122424 (8)	0.286321 (17)	0.01340 (7)
S1	0.12267 (13)	0.27684 (4)	0.41444 (9)	0.01958 (15)
O1	−0.0465 (4)	0.22556 (14)	0.3774 (3)	0.0271 (5)
O2	0.3081 (4)	0.23889 (14)	0.3843 (3)	0.0272 (5)
O3	0.0903 (5)	0.34036 (14)	0.3206 (3)	0.0310 (6)
O4	0.1364 (6)	0.29581 (15)	0.5766 (3)	0.0380 (7)
S2	−0.31329 (12)	0.07620 (5)	0.26382 (12)	0.02485 (18)
O21	−0.1631 (4)	0.0782 (2)	0.4041 (4)	0.0446 (9)
O22	−0.2053 (4)	0.11047 (19)	0.1446 (3)	0.0364 (7)
O23	−0.3710 (6)	0.00438 (19)	0.2278 (7)	0.0714 (15)
O24	−0.4892 (4)	0.11915 (15)	0.2885 (4)	0.0332 (6)
O5	0.2464 (5)	0.10893 (16)	0.5677 (3)	0.0354 (7)
H5A	0.2760	0.0708	0.6001	0.053*
H5B	0.1959	0.1347	0.6201	0.053*
O6	0.1923 (6)	−0.00455 (15)	0.3348 (4)	0.0396 (7)
H6A	0.2693	−0.0229	0.2902	0.059*
H6B	0.1780	−0.0252	0.4252	0.059*
O7	0.1693 (5)	0.05489 (15)	0.0409 (3)	0.0333 (6)
H7A	0.1227	0.0799	−0.0408	0.050*
H7B	0.2792	0.0380	0.0318	0.050*
N1	−0.3460 (6)	0.2224 (2)	−0.3854 (5)	0.0449 (10)
H1A	−0.4578	0.2226	−0.4626	0.067*
H1B	−0.3495	0.1791	−0.3198	0.067*
H1C	−0.3137	0.2658	−0.3492	0.067*
H1D	−0.2640	0.2109	−0.4701	0.067*
O8	−0.3625 (6)	0.1094 (2)	−0.1641 (4)	0.0480 (9)
H8A	−0.2909	0.1178	−0.0678	0.072*
H8B	−0.4731	0.0867	−0.1588	0.072*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Nd1	0.01172 (9)	0.01511 (9)	0.01366 (9)	0.00097 (5)	0.00271 (5)	0.00105 (5)
S1	0.0275 (4)	0.0168 (3)	0.0144 (3)	0.0047 (3)	0.0026 (3)	−0.0021 (3)
O1	0.0222 (12)	0.0265 (12)	0.0335 (13)	0.0034 (10)	0.0075 (10)	−0.0054 (10)
O2	0.0210 (12)	0.0253 (12)	0.0341 (14)	0.0036 (10)	−0.0015 (10)	−0.0089 (10)
O3	0.0481 (17)	0.0230 (12)	0.0225 (12)	0.0073 (12)	0.0064 (11)	0.0052 (10)
O4	0.078 (2)	0.0222 (12)	0.0145 (11)	0.0066 (14)	0.0064 (13)	−0.0046 (10)
S2	0.0131 (3)	0.0189 (4)	0.0441 (5)	−0.0005 (3)	0.0097 (3)	−0.0029 (3)
O21	0.0226 (13)	0.063 (2)	0.0486 (18)	0.0008 (14)	0.0060 (12)	0.0348 (17)
O22	0.0208 (12)	0.069 (2)	0.0194 (12)	−0.0113 (13)	0.0033 (10)	−0.0011 (13)
O23	0.0378 (19)	0.0303 (17)	0.150 (5)	−0.0113 (15)	0.027 (2)	−0.033 (2)
O24	0.0153 (11)	0.0305 (14)	0.0546 (18)	0.0046 (10)	0.0072 (11)	−0.0069 (13)
O5	0.0485 (18)	0.0382 (15)	0.0191 (12)	0.0166 (13)	0.0022 (12)	−0.0006 (11)
O6	0.065 (2)	0.0235 (13)	0.0345 (15)	0.0103 (14)	0.0223 (15)	0.0074 (11)
O7	0.0471 (17)	0.0287 (13)	0.0254 (13)	0.0095 (12)	0.0094 (12)	−0.0016 (11)
N1	0.040 (2)	0.053 (2)	0.038 (2)	−0.0120 (18)	−0.0095 (16)	0.0053 (18)
O8	0.0452 (19)	0.059 (2)	0.0365 (17)	−0.0136 (16)	−0.0085 (14)	−0.0002 (15)

Geometric parameters (Å, º)

Nd1—O4^i	2.402 (3)	S2—O24	1.461 (3)
Nd1—O24^ii	2.414 (3)	S2—O21	1.487 (3)
Nd1—O6	2.454 (3)	S2—O22	1.489 (3)
Nd1—O5	2.494 (3)	O24—Nd1^iv	2.414 (3)
Nd1—O22	2.519 (3)	O5—H5A	0.7919
Nd1—O1	2.520 (3)	O5—H5B	0.7746
Nd1—O7	2.527 (3)	O6—H6A	0.7638
Nd1—O21	2.554 (3)	O6—H6B	0.9015
Nd1—O2	2.554 (3)	O7—H7A	0.8842
Nd1—S1	3.1443 (8)	O7—H7B	0.8092
Nd1—S2	3.1586 (9)	N1—H1A	0.9417
S1—O3	1.459 (3)	N1—H1B	1.0033
S1—O4	1.462 (3)	N1—H1C	0.8992
S1—O2	1.477 (3)	N1—H1D	0.9981
S1—O1	1.490 (3)	O8—H8A	0.9319
O4—Nd1^iii	2.402 (3)	O8—H8B	0.8568
S2—O23	1.437 (3)
O4^i—Nd1—O24^ii	87.53 (12)	O22—Nd1—S2	27.58 (7)
O4^i—Nd1—O6	139.11 (10)	O1—Nd1—S2	73.08 (6)
O24^ii—Nd1—O6	82.62 (11)	O7—Nd1—S2	87.96 (8)
O4^i—Nd1—O5	143.74 (10)	O21—Nd1—S2	27.69 (8)
O24^ii—Nd1—O5	81.16 (11)	O2—Nd1—S2	128.48 (6)
O6—Nd1—O5	73.47 (10)	S1—Nd1—S2	100.88 (2)
O4^i—Nd1—O22	75.00 (11)	O3—S1—O4	109.62 (16)
O24^ii—Nd1—O22	150.22 (10)	O3—S1—O2	111.58 (17)
O6—Nd1—O22	94.86 (12)	O4—S1—O2	109.94 (18)
O5—Nd1—O22	126.73 (10)	O3—S1—O1	111.04 (17)
O4^i—Nd1—O1	77.10 (10)	O4—S1—O1	109.16 (18)
O24^ii—Nd1—O1	124.41 (9)	O2—S1—O1	105.42 (15)
O6—Nd1—O1	139.53 (9)	O3—S1—Nd1	125.05 (11)
O5—Nd1—O1	81.23 (9)	O4—S1—Nd1	125.30 (12)
O22—Nd1—O1	75.49 (10)	O2—S1—Nd1	53.36 (10)
O4^i—Nd1—O7	70.75 (9)	O1—S1—Nd1	52.10 (10)
O24^ii—Nd1—O7	80.20 (10)	S1—O1—Nd1	100.09 (12)
O6—Nd1—O7	68.49 (10)	S1—O2—Nd1	99.00 (13)
O5—Nd1—O7	139.31 (9)	S1—O4—Nd1^iii	154.06 (17)
O22—Nd1—O7	71.41 (10)	O23—S2—O24	111.31 (19)
O1—Nd1—O7	138.50 (9)	O23—S2—O21	109.9 (3)
O4^i—Nd1—O21	125.01 (11)	O24—S2—O21	109.2 (2)
O24^ii—Nd1—O21	147.46 (10)	O23—S2—O22	113.3 (3)
O6—Nd1—O21	72.36 (11)	O24—S2—O22	108.94 (19)
O5—Nd1—O21	72.13 (11)	O21—S2—O22	103.92 (16)
O22—Nd1—O21	55.04 (10)	O23—S2—Nd1	120.34 (15)
O1—Nd1—O21	70.04 (11)	O24—S2—Nd1	128.34 (12)
O7—Nd1—O21	108.37 (12)	O21—S2—Nd1	52.93 (11)
O4^i—Nd1—O2	70.94 (9)	O22—S2—Nd1	51.54 (11)
O24^ii—Nd1—O2	69.01 (9)	S2—O21—Nd1	99.39 (15)
O6—Nd1—O2	138.57 (10)	S2—O22—Nd1	100.88 (14)
O5—Nd1—O2	72.84 (10)	S2—O24—Nd1^iv	146.13 (17)
O22—Nd1—O2	124.69 (10)	Nd1—O5—H5A	118.2
O1—Nd1—O2	55.43 (8)	Nd1—O5—H5B	116.3
O7—Nd1—O2	131.16 (10)	H5A—O5—H5B	117.9
O21—Nd1—O2	118.11 (11)	Nd1—O6—H6A	115.6
O4^i—Nd1—S1	71.19 (7)	Nd1—O6—H6B	123.6
O24^ii—Nd1—S1	96.65 (7)	H6A—O6—H6B	113.9
O6—Nd1—S1	149.27 (8)	Nd1—O7—H7A	111.7
O5—Nd1—S1	76.05 (7)	Nd1—O7—H7B	115.6
O22—Nd1—S1	100.12 (8)	H7A—O7—H7B	111.1
O1—Nd1—S1	27.80 (6)	H1A—N1—H1B	110.3
O7—Nd1—S1	141.91 (7)	H1A—N1—H1C	112.5
O21—Nd1—S1	94.62 (9)	H1B—N1—H1C	124.4
O2—Nd1—S1	27.64 (6)	H1A—N1—H1D	85.3
O4^i—Nd1—S2	101.21 (9)	H1B—N1—H1D	107.7
O24^ii—Nd1—S2	162.15 (7)	H1C—N1—H1D	109.5
O6—Nd1—S2	80.62 (9)	H8A—O8—H8B	112.4
O5—Nd1—S2	99.80 (8)

Symmetry codes: (i) x, −y+1/2, z−1/2; (ii) x+1, y, z; (iii) x, −y+1/2, z+1/2; (iv) x−1, y, z.

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
O5—H5A···O23^v	0.79	2.12	2.855 (6)	155
O5—H5B···O3^iii	0.77	2.03	2.739 (4)	152
O6—H6A···O8^vi	0.76	2.11	2.808 (5)	151
O6—H6A···O23^ii	0.76	2.57	3.159 (5)	136
O6—H6B···O21^v	0.90	1.82	2.713 (4)	172
O7—H7A···O3^i	0.88	1.93	2.777 (4)	159
O7—H7B···O23^vi	0.81	2.56	3.067 (5)	122
N1—H1A···O2^vii	0.94	1.95	2.884 (5)	171
N1—H1B···O8	1.00	1.91	2.902 (6)	169
N1—H1C···O22^i	0.90	2.45	3.302 (6)	158
N1—H1C···O1^i	0.90	2.50	3.022 (5)	117
N1—H1D···O1^viii	1.00	2.11	3.053 (5)	158
O8—H8A···O22	0.93	1.89	2.785 (4)	161
O8—H8B···O23^ix	0.86	2.06	2.800 (5)	144

Symmetry codes: (i) x, −y+1/2, z−1/2; (ii) x+1, y, z; (iii) x, −y+1/2, z+1/2; (v) −x, −y, −z+1; (vi) −x, −y, −z; (vii) x−1, y, z−1; (viii) x, y, z−1; (ix) −x−1, −y, −z.