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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.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806047416/sg2089sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536806047416/sg2089Isup2.hkl
Contains datablock I

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

Computing details top

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 top
Crystal data top
Th(CrO4)2(H2O)F(000) = 3360
Mr = 480.04Dx = 4.432 Mg m3
Orthorhombic, PbcaMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ac 2abCell parameters from 3378 reflections
a = 10.9824 (6) Åθ = 1.8–28.3°
b = 11.6668 (6) ŵ = 23.60 mm1
c = 22.4586 (12) ÅT = 193 K
V = 2877.6 (3) Å3Distorted octahedron, dark red
Z = 160.10 × 0.09 × 0.09 mm
Data collection top
Bruker APEX
diffractometer
3581 independent reflections
Radiation source: fine-focus sealed tube3378 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.041
ω scansθmax = 28.3°, θmin = 1.8°
Absorption correction: numerical
(SHELXL97; Sheldrick, 1997)
h = 1414
Tmin = 0.116, Tmax = 0.124k = 1515
27721 measured reflectionsl = 2929
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.023H-atom parameters not defined
wR(F2) = 0.054 w = 1/[σ2(Fo2) + (0.0198P)2 + 22.6366P]
where P = (Fo2 + 2Fc2)/3
S = 1.11(Δ/σ)max = 0.001
3581 reflectionsΔρmax = 2.28 e Å3
217 parametersΔρmin = 1.09 e Å3
0 restraints
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
xyzUiso*/Ueq
Th10.138294 (17)0.713478 (16)0.052600 (8)0.00956 (6)
Th20.302282 (17)0.913318 (16)0.204540 (8)0.00900 (6)
Cr10.21600 (8)0.66059 (7)0.09005 (4)0.00960 (16)
Cr20.06510 (8)0.38313 (7)0.08362 (4)0.00973 (16)
Cr30.02982 (8)0.95739 (7)0.14273 (4)0.01053 (16)
Cr40.42307 (8)0.64236 (7)0.27894 (4)0.00987 (16)
O10.0724 (4)0.6959 (4)0.07938 (19)0.0190 (9)
O20.2786 (4)0.7526 (4)0.13583 (18)0.0177 (8)
O30.2852 (4)0.6642 (4)0.02415 (18)0.0178 (8)
O40.2223 (4)0.5298 (3)0.11736 (18)0.0172 (8)
O50.1130 (4)0.5071 (4)0.0578 (2)0.0226 (10)
O60.0086 (4)0.4016 (4)0.14601 (18)0.0171 (8)
O70.0251 (4)0.3222 (4)0.03445 (19)0.0262 (10)
O80.1825 (4)0.2983 (4)0.09675 (19)0.0191 (9)
O90.0746 (4)0.8948 (3)0.07693 (18)0.0160 (8)
O100.1386 (4)0.9455 (4)0.19332 (18)0.0169 (8)
O110.0035 (4)1.0890 (3)0.1301 (2)0.0209 (9)
O120.0949 (4)0.8942 (3)0.16795 (18)0.0146 (8)
O130.4378 (3)0.7625 (3)0.23987 (17)0.0132 (8)
O140.5576 (4)0.5844 (3)0.28525 (18)0.0179 (9)
O150.3275 (4)0.5575 (4)0.24503 (19)0.0190 (8)
O160.3651 (4)0.6743 (4)0.34557 (18)0.0180 (8)
O170.3206 (5)0.6025 (4)0.0126 (3)0.0365 (13)
O180.1813 (4)0.7951 (3)0.27252 (18)0.0155 (8)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Th10.01003 (9)0.01091 (10)0.00775 (9)0.00139 (7)0.00001 (6)0.00002 (6)
Th20.00918 (9)0.00950 (10)0.00833 (9)0.00036 (6)0.00011 (6)0.00022 (6)
Cr10.0104 (4)0.0104 (4)0.0080 (4)0.0002 (3)0.0004 (3)0.0006 (3)
Cr20.0095 (4)0.0106 (4)0.0091 (4)0.0005 (3)0.0000 (3)0.0002 (3)
Cr30.0109 (4)0.0115 (4)0.0091 (4)0.0009 (3)0.0006 (3)0.0000 (3)
Cr40.0112 (4)0.0099 (4)0.0085 (4)0.0008 (3)0.0000 (3)0.0005 (3)
O10.015 (2)0.024 (2)0.018 (2)0.0042 (16)0.0041 (16)0.0030 (17)
O20.018 (2)0.018 (2)0.018 (2)0.0005 (17)0.0028 (16)0.0050 (16)
O30.023 (2)0.016 (2)0.0144 (19)0.0038 (17)0.0039 (16)0.0026 (15)
O40.022 (2)0.016 (2)0.0144 (19)0.0004 (17)0.0005 (16)0.0030 (15)
O50.028 (2)0.013 (2)0.028 (2)0.0043 (18)0.0091 (19)0.0015 (17)
O60.019 (2)0.019 (2)0.0131 (19)0.0014 (16)0.0056 (16)0.0027 (16)
O70.030 (2)0.036 (3)0.012 (2)0.016 (2)0.0070 (18)0.0024 (18)
O80.015 (2)0.021 (2)0.021 (2)0.0062 (16)0.0010 (16)0.0025 (17)
O90.021 (2)0.0144 (19)0.0126 (19)0.0032 (16)0.0030 (16)0.0005 (15)
O100.015 (2)0.021 (2)0.0140 (19)0.0005 (16)0.0003 (15)0.0010 (16)
O110.024 (2)0.013 (2)0.027 (2)0.0044 (16)0.0030 (18)0.0003 (17)
O120.0115 (18)0.0162 (19)0.0161 (19)0.0017 (15)0.0038 (15)0.0001 (15)
O130.0112 (18)0.0144 (19)0.0138 (18)0.0043 (15)0.0006 (14)0.0019 (15)
O140.019 (2)0.019 (2)0.0154 (19)0.0062 (16)0.0014 (16)0.0046 (16)
O150.019 (2)0.021 (2)0.016 (2)0.0063 (17)0.0006 (16)0.0031 (17)
O160.018 (2)0.026 (2)0.0093 (18)0.0047 (18)0.0013 (15)0.0009 (16)
O170.023 (2)0.021 (2)0.066 (4)0.008 (2)0.018 (3)0.005 (2)
O180.0133 (18)0.018 (2)0.0152 (19)0.0008 (15)0.0028 (15)0.0040 (16)
Geometric parameters (Å, º) top
Th1—O92.294 (4)Cr2—O61.632 (4)
Th1—O16i2.332 (4)Cr2—O51.644 (4)
Th1—O7ii2.354 (4)Cr2—O71.645 (4)
Th1—O3iii2.390 (4)Cr2—O81.652 (4)
Th1—O12.400 (4)Cr3—O111.588 (4)
Th1—O8iv2.416 (4)Cr3—O101.655 (4)
Th1—O52.427 (4)Cr3—O121.655 (4)
Th1—O172.548 (5)Cr3—O91.720 (4)
Th2—O15v2.385 (4)Cr4—O141.631 (4)
Th2—O4v2.398 (4)Cr4—O151.632 (4)
Th2—O10vi2.413 (4)Cr4—O131.661 (4)
Th2—O122.432 (4)Cr4—O161.668 (4)
Th2—O132.438 (4)O3—Th1viii2.390 (4)
Th2—O22.442 (4)O4—Th2ix2.398 (4)
Th2—O182.450 (4)O6—Th2ix2.462 (4)
Th2—O6v2.462 (4)O7—Th1ii2.354 (4)
Th2—O14vii2.530 (4)O8—Th1x2.415 (4)
Cr1—O21.638 (4)O10—Th2i2.413 (4)
Cr1—O41.646 (4)O14—Th2xi2.530 (4)
Cr1—O11.647 (4)O15—Th2ix2.385 (4)
Cr1—O31.664 (4)O16—Th1vi2.333 (4)
O9—Th1—O16i86.69 (15)O12—Th2—O6v127.22 (13)
O9—Th1—O7ii101.52 (17)O13—Th2—O6v67.57 (13)
O16i—Th1—O7ii140.46 (15)O2—Th2—O6v73.14 (14)
O9—Th1—O3iii74.25 (14)O18—Th2—O6v139.39 (14)
O16i—Th1—O3iii146.08 (14)O15v—Th2—O14vii76.85 (15)
O7ii—Th1—O3iii72.07 (15)O4v—Th2—O14vii72.27 (14)
O9—Th1—O174.04 (15)O10vi—Th2—O14vii68.15 (14)
O16i—Th1—O173.86 (14)O12—Th2—O14vii132.24 (14)
O7ii—Th1—O171.56 (16)O13—Th2—O14vii99.71 (14)
O3iii—Th1—O1124.79 (15)O2—Th2—O14vii136.69 (14)
O9—Th1—O8iv76.88 (15)O18—Th2—O14vii135.86 (13)
O16i—Th1—O8iv71.99 (14)O6v—Th2—O14vii65.12 (14)
O7ii—Th1—O8iv147.53 (15)O2—Cr1—O4110.9 (2)
O3iii—Th1—O8iv76.43 (14)O2—Cr1—O1109.2 (2)
O1—Th1—O8iv135.87 (15)O4—Cr1—O1109.0 (2)
O9—Th1—O5150.28 (15)O2—Cr1—O3110.5 (2)
O16i—Th1—O575.90 (15)O4—Cr1—O3109.6 (2)
O7ii—Th1—O578.70 (16)O1—Cr1—O3107.6 (2)
O3iii—Th1—O5131.87 (14)O6—Cr2—O5110.2 (2)
O1—Th1—O578.03 (15)O6—Cr2—O7109.6 (2)
O8iv—Th1—O5118.68 (15)O5—Cr2—O7109.6 (2)
O9—Th1—O17142.40 (15)O6—Cr2—O8108.2 (2)
O16i—Th1—O17104.99 (17)O5—Cr2—O8109.9 (2)
O7ii—Th1—O1791.86 (19)O7—Cr2—O8109.3 (2)
O3iii—Th1—O1776.89 (16)O11—Cr3—O10109.6 (2)
O1—Th1—O17143.38 (16)O11—Cr3—O12110.0 (2)
O8iv—Th1—O1773.30 (17)O10—Cr3—O12109.0 (2)
O5—Th1—O1766.59 (16)O11—Cr3—O9108.0 (2)
O15v—Th2—O4v81.06 (14)O10—Cr3—O9110.4 (2)
O15v—Th2—O10vi71.86 (14)O12—Cr3—O9110.0 (2)
O4v—Th2—O10vi135.91 (14)O14—Cr4—O15111.8 (2)
O15v—Th2—O1268.51 (14)O14—Cr4—O13107.9 (2)
O4v—Th2—O1270.77 (14)O15—Cr4—O13109.2 (2)
O10vi—Th2—O12125.97 (14)O14—Cr4—O16111.1 (2)
O15v—Th2—O13138.59 (14)O15—Cr4—O16108.0 (2)
O4v—Th2—O13138.01 (13)O13—Cr4—O16108.8 (2)
O10vi—Th2—O1368.81 (13)Cr1—O1—Th1168.8 (2)
O12—Th2—O13128.02 (13)Cr1—O2—Th2160.9 (2)
O15v—Th2—O2135.94 (14)Cr1—O3—Th1viii144.8 (2)
O4v—Th2—O284.67 (14)Cr1—O4—Th2ix145.5 (2)
O10vi—Th2—O2138.47 (14)Cr2—O5—Th1157.9 (3)
O12—Th2—O267.44 (13)Cr2—O6—Th2ix152.1 (2)
O13—Th2—O273.53 (14)Cr2—O7—Th1ii162.2 (3)
O15v—Th2—O1880.53 (14)Cr2—O8—Th1x143.9 (2)
O4v—Th2—O18140.08 (14)Cr3—O9—Th1133.1 (2)
O10vi—Th2—O1868.96 (14)Cr3—O10—Th2i149.3 (2)
O12—Th2—O1869.57 (13)Cr3—O12—Th2148.2 (2)
O13—Th2—O1873.85 (13)Cr4—O13—Th2136.2 (2)
O2—Th2—O1884.46 (14)Cr4—O14—Th2xi152.3 (2)
O15v—Th2—O6v138.33 (15)Cr4—O15—Th2ix172.1 (3)
O4v—Th2—O6v71.96 (14)Cr4—O16—Th1vi158.3 (2)
O10vi—Th2—O6v106.81 (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) x1/2, y+1/2, z; (vi) x1/2, y, z+1/2; (vii) x1, y+1/2, z+1/2; (viii) x1/2, y+3/2, z; (ix) x1/2, y1/2, z; (x) x+1/2, y1/2, z; (xi) x1, y1/2, z+1/2.
 

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