Samarium(III) carbonate hydroxide

Sm(CO₃)(OH) was obtained hydro­thermally from an aqueous solution of samarium oxide, formic acid, triethyl­enetetra­mine and dimethyl­formamide. The structure features deca­coordinated samarium (site symmetry m) with carbonate and hydroxide acting as bridging ligands.

Key indicators

• Single-crystal X-ray study
• T = 293 K
• Mean [sigma](O-C) = 0.007 Å
• R factor = 0.047
• wR factor = 0.122
• Data-to-parameter ratio = 10.3

checkCIF/PLATON results

No syntax errors found



Alert level C
PLAT062_ALERT_4_C Rescale T(min) & T(max) by .....................       0.85
PLAT199_ALERT_1_C Check the Reported _cell_measurement_temperature        293 K
PLAT200_ALERT_1_C Check the Reported _diffrn_ambient_temperature .        293 K
PLAT764_ALERT_4_C Overcomplete CIF Bond List Detected (Rep/Expd) .       1.75 Ratio

Alert level G
ABSTM02_ALERT_3_G  When printed, the submitted absorption T values will be
            replaced by the scaled T values. Since the ratio of scaled T's
            is identical to the ratio of reported T values, the scaling
            does not imply a change to the absorption corrections used in
            the study.
            Ratio of Tmax expected/reported      0.853
            Tmax scaled      0.378 Tmin scaled      0.331

   0 ALERT level A = In general: serious problem
   0 ALERT level B = Potentially serious problem
   4 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
   0 ALERT type 2 Indicator that the structure model may be wrong or deficient
   1 ALERT type 3 Indicator that the structure quality may be low
   2 ALERT type 4 Improvement, methodology, query or suggestion

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Computing details

Data collection: APEX2 (Bruker, 2005); cell refinement: SAINT (Bruker, 2005); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997b); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997b); molecular graphics: SHELXTL (Sheldrick, 1997a); software used to prepare material for publication: SHELXTL.

Samarium(III) carbonate hydroxide

Crystal data

Sm(CO3)(OH)	F(000) = 404
Mr = 227.37	Dx = 5.052 Mg m^−3
Orthorhombic, Pnma	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ac 2n	Cell parameters from 1391 reflections
a = 7.161 (6) Å	θ = 3.7–27.0°
b = 4.929 (4) Å	µ = 19.46 mm^−1
c = 8.470 (7) Å	T = 293 K
V = 299.0 (4) Å^3	Block, yellow
Z = 4	0.06 × 0.05 × 0.05 mm

Data collection

Bruker APEX-2 CCD diffractometer	402 independent reflections
Radiation source: fine-focus sealed tube	374 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.060
ω scans	θmax = 28.0°, θmin = 3.7°
Absorption correction: multi-scan (SADABS; Sheldrick, 2003)	h = −5→9
Tmin = 0.388, Tmax = 0.443	k = −6→6
1471 measured reflections	l = −11→8

Refinement

Refinement on F^2	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.047	All H-atom parameters refined
wR(F^2) = 0.122	w = 1/[σ^2(Fo^2) + (0.0822P)^2] where P = (Fo^2 + 2Fc^2)/3
S = 1.17	(Δ/σ)max = 0.023
402 reflections	Δρmax = 3.90 e Å^−3
39 parameters	Δρmin = −3.98 e Å^−3
20 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: 0.0121 (10)

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	Occ. (<1)
Sm1	0.35871 (4)	0.2500	0.66569 (3)	0.00519 (10)
O1	0.1541 (4)	−0.0251 (8)	0.8892 (4)	0.0085 (4)
O2	0.2956 (7)	−0.2500	0.6978 (6)	0.0107 (11)
C1	0.1998 (10)	−0.2500	0.8231 (6)	0.0067 (5)
O3	0.5392 (5)	0.2500	0.8924 (3)	0.0069 (4)
H1	0.4979 (9)	0.1441 (10)	0.9684 (4)	0.010*	0.50

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Sm1	0.00909 (19)	0.0048 (2)	0.00173 (19)	0.000	−0.00074 (9)	0.000
O1	0.0093 (6)	0.0079 (6)	0.0082 (6)	0.0000 (5)	−0.0006 (5)	−0.0006 (5)
O2	0.012 (2)	0.013 (2)	0.0074 (17)	0.000	0.0033 (19)	0.000
C1	0.0066 (7)	0.0069 (7)	0.0065 (7)	0.000	0.0001 (5)	0.000
O3	0.0068 (6)	0.0074 (7)	0.0064 (7)	0.000	0.0000 (5)	0.000

Geometric parameters (Å, º)

Sm1—O3	2.315 (3)	Sm1—C1	3.024 (4)
Sm1—O3^i	2.340 (4)	O1—C1	1.284 (5)
Sm1—O2	2.520 (2)	O1—Sm1^i	2.555 (3)
Sm1—O2^ii	2.520 (2)	O1—Sm1^viii	2.593 (4)
Sm1—O1^iii	2.555 (3)	O2—C1	1.263 (8)
Sm1—O1^iv	2.555 (3)	O2—Sm1^ix	2.520 (2)
Sm1—O1^v	2.593 (4)	C1—O1^x	1.284 (5)
Sm1—O1^vi	2.593 (4)	C1—Sm1^viii	2.932 (6)
Sm1—O1^vii	2.751 (4)	C1—Sm1^ix	3.024 (4)
Sm1—O1	2.751 (4)	O3—Sm1^iv	2.340 (4)
Sm1—C1^v	2.932 (6)	O3—H1	0.880 (3)
O3—Sm1—O3^i	136.08 (10)	O2—Sm1—C1^v	94.66 (11)
O3—Sm1—O2	90.60 (11)	O2^ii—Sm1—C1^v	94.66 (11)
O3^i—Sm1—O2	81.23 (12)	O1^iii—Sm1—C1^v	86.46 (15)
O3—Sm1—O2^ii	90.60 (11)	O1^iv—Sm1—C1^v	86.46 (15)
O3^i—Sm1—O2^ii	81.23 (12)	O1^v—Sm1—C1^v	25.96 (9)
O2—Sm1—O2^ii	155.8 (2)	O1^vi—Sm1—C1^v	25.96 (9)
O3—Sm1—O1^iii	71.86 (11)	O1^vii—Sm1—C1^v	127.22 (14)
O3^i—Sm1—O1^iii	140.45 (10)	O1—Sm1—C1^v	127.22 (14)
O2—Sm1—O1^iii	133.39 (14)	O3—Sm1—C1	81.04 (13)
O2^ii—Sm1—O1^iii	69.46 (15)	O3^i—Sm1—C1	74.03 (14)
O3—Sm1—O1^iv	71.86 (11)	O2—Sm1—C1	24.23 (14)
O3^i—Sm1—O1^iv	140.45 (10)	O2^ii—Sm1—C1	132.98 (15)
O2—Sm1—O1^iv	69.46 (14)	O1^iii—Sm1—C1	145.49 (16)
O2^ii—Sm1—O1^iv	133.39 (14)	O1^iv—Sm1—C1	87.66 (15)
O1^iii—Sm1—O1^iv	64.10 (18)	O1^v—Sm1—C1	92.10 (13)
O3—Sm1—O1^v	140.27 (10)	O1^vi—Sm1—C1	137.17 (14)
O3^i—Sm1—O1^v	77.03 (9)	O1^vii—Sm1—C1	84.13 (14)
O2—Sm1—O1^v	70.92 (14)	O1—Sm1—C1	25.13 (12)
O2^ii—Sm1—O1^v	120.62 (14)	C1^v—Sm1—C1	112.49 (9)
O1^iii—Sm1—O1^v	95.26 (8)	C1—O1—Sm1^i	126.2 (4)
O1^iv—Sm1—O1^v	68.78 (12)	C1—O1—Sm1^viii	91.9 (3)
O3—Sm1—O1^vi	140.27 (10)	Sm1^i—O1—Sm1^viii	111.22 (12)
O3^i—Sm1—O1^vi	77.03 (9)	C1—O1—Sm1	89.4 (3)
O2—Sm1—O1^vi	120.62 (14)	Sm1^i—O1—Sm1	93.11 (13)
O2^ii—Sm1—O1^vi	70.92 (14)	Sm1^viii—O1—Sm1	148.32 (12)
O1^iii—Sm1—O1^vi	68.78 (12)	C1—O2—Sm1	100.84 (11)
O1^iv—Sm1—O1^vi	95.26 (8)	C1—O2—Sm1^ix	100.84 (11)
O1^v—Sm1—O1^vi	50.62 (18)	Sm1—O2—Sm1^ix	155.8 (2)
O3—Sm1—O1^vii	74.13 (11)	O2—C1—O1	120.3 (3)
O3^i—Sm1—O1^vii	67.91 (9)	O2—C1—O1^x	120.3 (3)
O2—Sm1—O1^vii	108.18 (14)	O1—C1—O1^x	119.3 (6)
O2^ii—Sm1—O1^vii	49.33 (13)	O2—C1—Sm1^viii	155.3 (5)
O1^iii—Sm1—O1^vii	107.74 (14)	O1—C1—Sm1^viii	62.1 (3)
O1^iv—Sm1—O1^vii	145.86 (7)	O1^x—C1—Sm1^viii	62.1 (3)
O1^v—Sm1—O1^vii	144.43 (6)	O2—C1—Sm1^ix	54.93 (11)
O1^vi—Sm1—O1^vii	113.08 (6)	O1—C1—Sm1^ix	172.5 (5)
O3—Sm1—O1	74.13 (11)	O1^x—C1—Sm1^ix	65.5 (2)
O3^i—Sm1—O1	67.91 (9)	Sm1^viii—C1—Sm1^ix	119.35 (12)
O2—Sm1—O1	49.33 (13)	O2—C1—Sm1	54.93 (11)
O2^ii—Sm1—O1	108.18 (14)	O1—C1—Sm1	65.5 (2)
O1^iii—Sm1—O1	145.86 (7)	O1^x—C1—Sm1	172.5 (5)
O1^iv—Sm1—O1	107.74 (14)	Sm1^viii—C1—Sm1	119.35 (12)
O1^v—Sm1—O1	113.08 (6)	Sm1^ix—C1—Sm1	109.2 (2)
O1^vi—Sm1—O1	144.43 (6)	Sm1—O3—Sm1^iv	111.80 (12)
O1^vii—Sm1—O1	59.04 (17)	Sm1—O3—H1	114.8 (4)
O3—Sm1—C1^v	154.28 (17)	Sm1^iv—O3—H1	118.9 (5)
O3^i—Sm1—C1^v	69.64 (16)

Symmetry codes: (i) x−1/2, y, −z+3/2; (ii) x, y+1, z; (iii) x+1/2, −y+1/2, −z+3/2; (iv) x+1/2, y, −z+3/2; (v) −x+1/2, −y, z−1/2; (vi) −x+1/2, y+1/2, z−1/2; (vii) x, −y+1/2, z; (viii) −x+1/2, −y, z+1/2; (ix) x, y−1, z; (x) x, −y−1/2, z.