Thorium(IV) chromate(VI) monohydrate

A new hydrated thorium chromate, Th(CrO₄)₂(H₂O), has been synthesized under mild hydro­thermal conditions. The structure consists of ThO₈ dodeca­hedra and ThO₉ tricapped trigonal prisms that are inter­connected by chromate anions into a three-dimensional framework.

Key indicators

• Single-crystal X-ray study
• T = 193 K
• Mean [sigma](r-O) = 0.004 Å
• R factor = 0.023
• wR factor = 0.054
• Data-to-parameter ratio = 16.5

checkCIF/PLATON results

No syntax errors found



Alert level C
PLAT094_ALERT_2_C Ratio of Maximum / Minimum Residual Density ....       2.09
PLAT220_ALERT_2_C Large Non-Solvent    O     Ueq(max)/Ueq(min) ...       2.80 Ratio

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

   0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
   2 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
   0 ALERT type 5 Informative message, check

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Computing details

Data collection: SMART (Bruker, 2000); cell refinement: SMART and SAINT (Bruker, 1999); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ATOMS (Dowty, 2004); software used to prepare material for publication: SHELXL97.

Thorium chromate monohydrate

Crystal data

Th(CrO4)2(H2O)	F(000) = 3360
Mr = 480.04	Dx = 4.432 Mg m^−3
Orthorhombic, Pbca	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ac 2ab	Cell parameters from 3378 reflections
a = 10.9824 (6) Å	θ = 1.8–28.3°
b = 11.6668 (6) Å	µ = 23.60 mm^−1
c = 22.4586 (12) Å	T = 193 K
V = 2877.6 (3) Å^3	Distorted octahedron, dark red
Z = 16	0.10 × 0.09 × 0.09 mm

Data collection

Bruker APEX diffractometer	3581 independent reflections
Radiation source: fine-focus sealed tube	3378 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.041
ω scans	θmax = 28.3°, θmin = 1.8°
Absorption correction: numerical (SHELXL97; Sheldrick, 1997)	h = −14→14
Tmin = 0.116, Tmax = 0.124	k = −15→15
27721 measured reflections	l = −29→29

Refinement

Refinement on F^2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.023	H-atom parameters not defined
wR(F^2) = 0.054	w = 1/[σ^2(Fo^2) + (0.0198P)^2 + 22.6366P] where P = (Fo^2 + 2Fc^2)/3
S = 1.11	(Δ/σ)max = 0.001
3581 reflections	Δρmax = 2.28 e Å^−3
217 parameters	Δρmin = −1.09 e Å^−3
0 restraints

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
Th1	0.138294 (17)	0.713478 (16)	0.052600 (8)	0.00956 (6)
Th2	−0.302282 (17)	0.913318 (16)	0.204540 (8)	0.00900 (6)
Cr1	−0.21600 (8)	0.66059 (7)	0.09005 (4)	0.00960 (16)
Cr2	0.06510 (8)	0.38313 (7)	0.08362 (4)	0.00973 (16)
Cr3	0.02982 (8)	0.95739 (7)	0.14273 (4)	0.01053 (16)
Cr4	−0.42307 (8)	0.64236 (7)	0.27894 (4)	0.00987 (16)
O1	−0.0724 (4)	0.6959 (4)	0.07938 (19)	0.0190 (9)
O2	−0.2786 (4)	0.7526 (4)	0.13583 (18)	0.0177 (8)
O3	−0.2852 (4)	0.6642 (4)	0.02415 (18)	0.0178 (8)
O4	−0.2223 (4)	0.5298 (3)	0.11736 (18)	0.0172 (8)
O5	0.1130 (4)	0.5071 (4)	0.0578 (2)	0.0226 (10)
O6	−0.0086 (4)	0.4016 (4)	0.14601 (18)	0.0171 (8)
O7	−0.0251 (4)	0.3222 (4)	0.03445 (19)	0.0262 (10)
O8	0.1825 (4)	0.2983 (4)	0.09675 (19)	0.0191 (9)
O9	0.0746 (4)	0.8948 (3)	0.07693 (18)	0.0160 (8)
O10	0.1386 (4)	0.9455 (4)	0.19332 (18)	0.0169 (8)
O11	0.0035 (4)	1.0890 (3)	0.1301 (2)	0.0209 (9)
O12	−0.0949 (4)	0.8942 (3)	0.16795 (18)	0.0146 (8)
O13	−0.4378 (3)	0.7625 (3)	0.23987 (17)	0.0132 (8)
O14	−0.5576 (4)	0.5844 (3)	0.28525 (18)	0.0179 (9)
O15	−0.3275 (4)	0.5575 (4)	0.24503 (19)	0.0190 (8)
O16	−0.3651 (4)	0.6743 (4)	0.34557 (18)	0.0180 (8)
O17	0.3206 (5)	0.6025 (4)	0.0126 (3)	0.0365 (13)
O18	−0.1813 (4)	0.7951 (3)	0.27252 (18)	0.0155 (8)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Th1	0.01003 (9)	0.01091 (10)	0.00775 (9)	−0.00139 (7)	0.00001 (6)	0.00002 (6)
Th2	0.00918 (9)	0.00950 (10)	0.00833 (9)	−0.00036 (6)	−0.00011 (6)	0.00022 (6)
Cr1	0.0104 (4)	0.0104 (4)	0.0080 (4)	0.0002 (3)	0.0004 (3)	0.0006 (3)
Cr2	0.0095 (4)	0.0106 (4)	0.0091 (4)	−0.0005 (3)	0.0000 (3)	0.0002 (3)
Cr3	0.0109 (4)	0.0115 (4)	0.0091 (4)	0.0009 (3)	0.0006 (3)	0.0000 (3)
Cr4	0.0112 (4)	0.0099 (4)	0.0085 (4)	−0.0008 (3)	0.0000 (3)	−0.0005 (3)
O1	0.015 (2)	0.024 (2)	0.018 (2)	−0.0042 (16)	0.0041 (16)	−0.0030 (17)
O2	0.018 (2)	0.018 (2)	0.018 (2)	−0.0005 (17)	0.0028 (16)	−0.0050 (16)
O3	0.023 (2)	0.016 (2)	0.0144 (19)	0.0038 (17)	−0.0039 (16)	0.0026 (15)
O4	0.022 (2)	0.016 (2)	0.0144 (19)	−0.0004 (17)	0.0005 (16)	0.0030 (15)
O5	0.028 (2)	0.013 (2)	0.028 (2)	−0.0043 (18)	0.0091 (19)	0.0015 (17)
O6	0.019 (2)	0.019 (2)	0.0131 (19)	0.0014 (16)	0.0056 (16)	−0.0027 (16)
O7	0.030 (2)	0.036 (3)	0.012 (2)	−0.016 (2)	−0.0070 (18)	0.0024 (18)
O8	0.015 (2)	0.021 (2)	0.021 (2)	0.0062 (16)	0.0010 (16)	0.0025 (17)
O9	0.021 (2)	0.0144 (19)	0.0126 (19)	0.0032 (16)	0.0030 (16)	−0.0005 (15)
O10	0.015 (2)	0.021 (2)	0.0140 (19)	−0.0005 (16)	−0.0003 (15)	−0.0010 (16)
O11	0.024 (2)	0.013 (2)	0.027 (2)	0.0044 (16)	0.0030 (18)	−0.0003 (17)
O12	0.0115 (18)	0.0162 (19)	0.0161 (19)	−0.0017 (15)	0.0038 (15)	−0.0001 (15)
O13	0.0112 (18)	0.0144 (19)	0.0138 (18)	−0.0043 (15)	−0.0006 (14)	0.0019 (15)
O14	0.019 (2)	0.019 (2)	0.0154 (19)	−0.0062 (16)	−0.0014 (16)	0.0046 (16)
O15	0.019 (2)	0.021 (2)	0.016 (2)	0.0063 (17)	−0.0006 (16)	−0.0031 (17)
O16	0.018 (2)	0.026 (2)	0.0093 (18)	−0.0047 (18)	−0.0013 (15)	−0.0009 (16)
O17	0.023 (2)	0.021 (2)	0.066 (4)	0.008 (2)	0.018 (3)	0.005 (2)
O18	0.0133 (18)	0.018 (2)	0.0152 (19)	0.0008 (15)	0.0028 (15)	0.0040 (16)

Geometric parameters (Å, º)

Th1—O9	2.294 (4)	Cr2—O6	1.632 (4)
Th1—O16^i	2.332 (4)	Cr2—O5	1.644 (4)
Th1—O7^ii	2.354 (4)	Cr2—O7	1.645 (4)
Th1—O3^iii	2.390 (4)	Cr2—O8	1.652 (4)
Th1—O1	2.400 (4)	Cr3—O11	1.588 (4)
Th1—O8^iv	2.416 (4)	Cr3—O10	1.655 (4)
Th1—O5	2.427 (4)	Cr3—O12	1.655 (4)
Th1—O17	2.548 (5)	Cr3—O9	1.720 (4)
Th2—O15^v	2.385 (4)	Cr4—O14	1.631 (4)
Th2—O4^v	2.398 (4)	Cr4—O15	1.632 (4)
Th2—O10^vi	2.413 (4)	Cr4—O13	1.661 (4)
Th2—O12	2.432 (4)	Cr4—O16	1.668 (4)
Th2—O13	2.438 (4)	O3—Th1^viii	2.390 (4)
Th2—O2	2.442 (4)	O4—Th2^ix	2.398 (4)
Th2—O18	2.450 (4)	O6—Th2^ix	2.462 (4)
Th2—O6^v	2.462 (4)	O7—Th1^ii	2.354 (4)
Th2—O14^vii	2.530 (4)	O8—Th1^x	2.415 (4)
Cr1—O2	1.638 (4)	O10—Th2^i	2.413 (4)
Cr1—O4	1.646 (4)	O14—Th2^xi	2.530 (4)
Cr1—O1	1.647 (4)	O15—Th2^ix	2.385 (4)
Cr1—O3	1.664 (4)	O16—Th1^vi	2.333 (4)
O9—Th1—O16^i	86.69 (15)	O12—Th2—O6^v	127.22 (13)
O9—Th1—O7^ii	101.52 (17)	O13—Th2—O6^v	67.57 (13)
O16^i—Th1—O7^ii	140.46 (15)	O2—Th2—O6^v	73.14 (14)
O9—Th1—O3^iii	74.25 (14)	O18—Th2—O6^v	139.39 (14)
O16^i—Th1—O3^iii	146.08 (14)	O15^v—Th2—O14^vii	76.85 (15)
O7^ii—Th1—O3^iii	72.07 (15)	O4^v—Th2—O14^vii	72.27 (14)
O9—Th1—O1	74.04 (15)	O10^vi—Th2—O14^vii	68.15 (14)
O16^i—Th1—O1	73.86 (14)	O12—Th2—O14^vii	132.24 (14)
O7^ii—Th1—O1	71.56 (16)	O13—Th2—O14^vii	99.71 (14)
O3^iii—Th1—O1	124.79 (15)	O2—Th2—O14^vii	136.69 (14)
O9—Th1—O8^iv	76.88 (15)	O18—Th2—O14^vii	135.86 (13)
O16^i—Th1—O8^iv	71.99 (14)	O6^v—Th2—O14^vii	65.12 (14)
O7^ii—Th1—O8^iv	147.53 (15)	O2—Cr1—O4	110.9 (2)
O3^iii—Th1—O8^iv	76.43 (14)	O2—Cr1—O1	109.2 (2)
O1—Th1—O8^iv	135.87 (15)	O4—Cr1—O1	109.0 (2)
O9—Th1—O5	150.28 (15)	O2—Cr1—O3	110.5 (2)
O16^i—Th1—O5	75.90 (15)	O4—Cr1—O3	109.6 (2)
O7^ii—Th1—O5	78.70 (16)	O1—Cr1—O3	107.6 (2)
O3^iii—Th1—O5	131.87 (14)	O6—Cr2—O5	110.2 (2)
O1—Th1—O5	78.03 (15)	O6—Cr2—O7	109.6 (2)
O8^iv—Th1—O5	118.68 (15)	O5—Cr2—O7	109.6 (2)
O9—Th1—O17	142.40 (15)	O6—Cr2—O8	108.2 (2)
O16^i—Th1—O17	104.99 (17)	O5—Cr2—O8	109.9 (2)
O7^ii—Th1—O17	91.86 (19)	O7—Cr2—O8	109.3 (2)
O3^iii—Th1—O17	76.89 (16)	O11—Cr3—O10	109.6 (2)
O1—Th1—O17	143.38 (16)	O11—Cr3—O12	110.0 (2)
O8^iv—Th1—O17	73.30 (17)	O10—Cr3—O12	109.0 (2)
O5—Th1—O17	66.59 (16)	O11—Cr3—O9	108.0 (2)
O15^v—Th2—O4^v	81.06 (14)	O10—Cr3—O9	110.4 (2)
O15^v—Th2—O10^vi	71.86 (14)	O12—Cr3—O9	110.0 (2)
O4^v—Th2—O10^vi	135.91 (14)	O14—Cr4—O15	111.8 (2)
O15^v—Th2—O12	68.51 (14)	O14—Cr4—O13	107.9 (2)
O4^v—Th2—O12	70.77 (14)	O15—Cr4—O13	109.2 (2)
O10^vi—Th2—O12	125.97 (14)	O14—Cr4—O16	111.1 (2)
O15^v—Th2—O13	138.59 (14)	O15—Cr4—O16	108.0 (2)
O4^v—Th2—O13	138.01 (13)	O13—Cr4—O16	108.8 (2)
O10^vi—Th2—O13	68.81 (13)	Cr1—O1—Th1	168.8 (2)
O12—Th2—O13	128.02 (13)	Cr1—O2—Th2	160.9 (2)
O15^v—Th2—O2	135.94 (14)	Cr1—O3—Th1^viii	144.8 (2)
O4^v—Th2—O2	84.67 (14)	Cr1—O4—Th2^ix	145.5 (2)
O10^vi—Th2—O2	138.47 (14)	Cr2—O5—Th1	157.9 (3)
O12—Th2—O2	67.44 (13)	Cr2—O6—Th2^ix	152.1 (2)
O13—Th2—O2	73.53 (14)	Cr2—O7—Th1^ii	162.2 (3)
O15^v—Th2—O18	80.53 (14)	Cr2—O8—Th1^x	143.9 (2)
O4^v—Th2—O18	140.08 (14)	Cr3—O9—Th1	133.1 (2)
O10^vi—Th2—O18	68.96 (14)	Cr3—O10—Th2^i	149.3 (2)
O12—Th2—O18	69.57 (13)	Cr3—O12—Th2	148.2 (2)
O13—Th2—O18	73.85 (13)	Cr4—O13—Th2	136.2 (2)
O2—Th2—O18	84.46 (14)	Cr4—O14—Th2^xi	152.3 (2)
O15^v—Th2—O6^v	138.33 (15)	Cr4—O15—Th2^ix	172.1 (3)
O4^v—Th2—O6^v	71.96 (14)	Cr4—O16—Th1^vi	158.3 (2)
O10^vi—Th2—O6^v	106.81 (14)

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