Copper(II) selenate pentahydrate is isotypic with its sulfate analogue. All atoms are on general positions except Cu1 and Cu2 (both with site symmetry
). The Jahn-Teller distortion of the CuO
2(H
2O)
4 `octahedra' is slightly less pronounced than in the sulfate analogue. The average Se-O bond length is 1.640 Å.
Supporting information
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (Se-O) = 0.001 Å
- R factor = 0.018
- wR factor = 0.047
- Data-to-parameter ratio = 15.2
checkCIF results
No syntax errors found
ADDSYM reports no extra symmetry
Alert Level C:
ABSTM_02 Alert C The ratio of expected to reported Tmax/Tmin(RR) is > 1.10
Tmin and Tmax reported: 0.233 0.437
Tmin and Tmax expected: 0.174 0.371
RR = 1.135
Please check that your absorption correction is appropriate.
PLAT_354 Alert C Short O-H Bond (0.82A) OW8 - H82 = 0.69 Ang.
General Notes
ABSTM_02 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 0.849
Tmax scaled 0.371 Tmin scaled 0.197
0 Alert Level A = Potentially serious problem
0 Alert Level B = Potential problem
2 Alert Level C = Please check
Data collection: COLLECT (Nonius, 2001); cell refinement: HKL, SCALEPACK (Otwinowski & Minor, 1997); data reduction: HKL, DENZO and SCALEPACK (Otwinowski & Minor, 1997); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997a); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997b); molecular graphics: ATOMS (Shape Software, 1999); software used to prepare material for publication: SHELXL97 (Sheldrick, 1997b).
'copper(II) selenate pentahydrate'
top
Crystal data top
CuH10O9Se | Z = 2 |
Mr = 296.58 | F(000) = 290 |
Triclinic, P1 | Dx = 2.576 Mg m−3 |
a = 6.083 (1) Å | Mo Kα radiation, λ = 0.71073 Å |
b = 6.226 (1) Å | Cell parameters from 3095 reflections |
c = 10.867 (2) Å | θ = 3.6–30.0° |
α = 77.14 (3)° | µ = 7.63 mm−1 |
β = 82.20 (3)° | T = 293 K |
γ = 72.91 (3)° | Fragment, pale blue |
V = 382.43 (11) Å3 | 0.27 × 0.20 × 0.13 mm |
Data collection top
Nonius KappaCCD diffractometer | 2194 independent reflections |
Radiation source: fine-focus sealed tube | 2115 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.012 |
ψ and ω scans | θmax = 30.0°, θmin = 3.5° |
Absorption correction: multi-scan (HKL, SCALEPACK; Otwinowski & Minor, 1997) | h = −8→8 |
Tmin = 0.233, Tmax = 0.437 | k = −7→8 |
4115 measured reflections | l = −15→15 |
Refinement top
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.018 | All H-atom parameters refined |
wR(F2) = 0.047 | w = 1/[σ2(Fo2) + (0.019P)2 + 0.220P] where P = (Fo2 + 2Fc2)/3 |
S = 1.10 | (Δ/σ)max = 0.001 |
2194 reflections | Δρmax = 0.49 e Å−3 |
144 parameters | Δρmin = −0.77 e Å−3 |
0 restraints | Extinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
Primary atom site location: structure-invariant direct methods | Extinction coefficient: 0.103 (2) |
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 | Uiso*/Ueq | |
Se | 0.11983 (2) | 0.99149 (2) | 0.786458 (13) | 0.01186 (7) | |
Cu1 | 0.5000 | 0.0000 | 0.5000 | 0.01508 (8) | |
Cu2 | 0.5000 | 0.5000 | 0.0000 | 0.01372 (8) | |
O1 | 0.1324 (2) | 0.1562 (2) | 0.88206 (13) | 0.0231 (3) | |
O2 | 0.1749 (2) | 0.1093 (2) | 0.63939 (12) | 0.0223 (3) | |
O3 | 0.3016 (2) | 0.7369 (2) | 0.81883 (12) | 0.0229 (3) | |
O4 | −0.1434 (2) | 0.9620 (2) | 0.80059 (12) | 0.0196 (2) | |
OW5 | 0.5168 (3) | 0.2441 (3) | 0.92351 (17) | 0.0302 (3) | |
OW6 | 0.2114 (2) | 0.4628 (3) | 0.09532 (16) | 0.0275 (3) | |
OW7 | 0.3523 (3) | 0.8181 (3) | 0.42929 (14) | 0.0239 (3) | |
OW8 | 0.3530 (3) | 0.2836 (2) | 0.38201 (13) | 0.0223 (3) | |
OW9 | 0.1239 (3) | 0.5730 (3) | 0.62223 (15) | 0.0260 (3) | |
H51 | 0.411 (6) | 0.222 (6) | 0.911 (3) | 0.049 (9)* | |
H52 | 0.630 (6) | 0.161 (5) | 0.895 (3) | 0.042 (8)* | |
H61 | 0.116 (5) | 0.570 (6) | 0.097 (3) | 0.040 (8)* | |
H62 | 0.181 (5) | 0.344 (6) | 0.117 (3) | 0.045 (8)* | |
H71 | 0.274 (5) | 0.749 (5) | 0.482 (3) | 0.038 (7)* | |
H72 | 0.278 (5) | 0.886 (6) | 0.370 (3) | 0.048 (9)* | |
H81 | 0.178 (8) | 0.351 (7) | 0.368 (4) | 0.090 (13)* | |
H82 | 0.415 (6) | 0.306 (5) | 0.325 (3) | 0.046 (9)* | |
H91 | 0.180 (5) | 0.584 (5) | 0.677 (3) | 0.044 (9)* | |
H92 | 0.159 (6) | 0.434 (6) | 0.624 (3) | 0.055 (10)* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Se | 0.01034 (9) | 0.01100 (10) | 0.01389 (9) | −0.00214 (6) | −0.00040 (6) | −0.00304 (6) |
Cu1 | 0.01494 (14) | 0.01619 (16) | 0.01447 (14) | −0.00458 (11) | −0.00295 (10) | −0.00216 (10) |
Cu2 | 0.01208 (14) | 0.01243 (15) | 0.01771 (14) | −0.00461 (10) | 0.00224 (10) | −0.00541 (10) |
O1 | 0.0189 (6) | 0.0260 (7) | 0.0293 (7) | −0.0044 (5) | −0.0037 (5) | −0.0166 (5) |
O2 | 0.0247 (6) | 0.0199 (6) | 0.0169 (6) | −0.0045 (5) | 0.0043 (5) | 0.0016 (5) |
O3 | 0.0234 (6) | 0.0160 (6) | 0.0213 (6) | 0.0059 (5) | −0.0032 (5) | −0.0017 (5) |
O4 | 0.0134 (5) | 0.0235 (6) | 0.0242 (6) | −0.0083 (5) | 0.0009 (5) | −0.0066 (5) |
OW5 | 0.0143 (6) | 0.0283 (8) | 0.0562 (10) | −0.0046 (6) | 0.0018 (6) | −0.0295 (7) |
OW6 | 0.0175 (6) | 0.0157 (7) | 0.0444 (9) | −0.0048 (6) | 0.0116 (6) | −0.0037 (6) |
OW7 | 0.0261 (7) | 0.0270 (7) | 0.0225 (6) | −0.0133 (6) | −0.0070 (6) | −0.0018 (5) |
OW8 | 0.0210 (6) | 0.0247 (7) | 0.0175 (6) | −0.0037 (5) | −0.0018 (5) | 0.0006 (5) |
OW9 | 0.0296 (7) | 0.0180 (7) | 0.0293 (8) | −0.0059 (6) | −0.0011 (6) | −0.0040 (5) |
Geometric parameters (Å, º) top
Se—O1i | 1.6368 (13) | O1—Seiii | 1.6368 (13) |
Se—O2i | 1.6375 (13) | O2—Seiii | 1.6375 (13) |
Se—O3 | 1.6386 (14) | O3—Cu2vii | 2.4115 (16) |
Se—O4 | 1.6479 (12) | OW5—Cu2vii | 1.9261 (14) |
Cu1—OW7ii | 1.9632 (14) | OW5—H51 | 0.73 (4) |
Cu1—OW7iii | 1.9632 (14) | OW5—H52 | 0.80 (3) |
Cu1—OW8iv | 1.9842 (16) | OW6—H61 | 0.75 (3) |
Cu1—OW8 | 1.9842 (16) | OW6—H62 | 0.79 (3) |
Cu1—O2iv | 2.3501 (15) | OW7—Cu1i | 1.9632 (14) |
Cu1—O2 | 2.3501 (15) | OW7—H71 | 0.83 (3) |
Cu2—OW5ii | 1.9261 (14) | OW7—H72 | 0.80 (3) |
Cu2—OW5v | 1.9261 (14) | OW8—H81 | 1.04 (4) |
Cu2—OW6vi | 1.9613 (15) | OW8—H82 | 0.69 (3) |
Cu2—OW6 | 1.9613 (15) | OW9—H91 | 0.75 (3) |
Cu2—O3ii | 2.4115 (16) | OW9—H92 | 0.82 (4) |
Cu2—O3v | 2.4115 (16) | | |
| | | |
O1i—Se—O2i | 110.30 (7) | OW6vi—Cu2—OW6 | 180.0 |
O1i—Se—O3 | 112.00 (7) | OW5ii—Cu2—O3ii | 86.21 (7) |
O2i—Se—O3 | 109.02 (7) | OW5v—Cu2—O3ii | 93.79 (7) |
O1i—Se—O4 | 108.81 (7) | OW6vi—Cu2—O3ii | 92.42 (6) |
O2i—Se—O4 | 108.03 (7) | OW6—Cu2—O3ii | 87.58 (6) |
O3—Se—O4 | 108.59 (7) | OW5ii—Cu2—O3v | 93.79 (7) |
OW7ii—Cu1—OW7iii | 180.0 | OW5v—Cu2—O3v | 86.21 (7) |
OW7ii—Cu1—OW8iv | 91.60 (6) | OW6vi—Cu2—O3v | 87.58 (6) |
OW7iii—Cu1—OW8iv | 88.40 (6) | OW6—Cu2—O3v | 92.42 (6) |
OW7ii—Cu1—OW8 | 88.40 (6) | O3ii—Cu2—O3v | 180.0 |
OW7iii—Cu1—OW8 | 91.60 (6) | Seiii—O2—Cu1 | 129.36 (8) |
OW8iv—Cu1—OW8 | 180.00 (7) | Se—O3—Cu2vii | 136.51 (8) |
OW7ii—Cu1—O2iv | 91.93 (6) | Cu2vii—OW5—H51 | 120 (3) |
OW7iii—Cu1—O2iv | 88.07 (6) | Cu2vii—OW5—H52 | 127 (2) |
OW8iv—Cu1—O2iv | 85.28 (6) | H51—OW5—H52 | 112 (3) |
OW8—Cu1—O2iv | 94.72 (6) | Cu2—OW6—H61 | 116 (2) |
OW7ii—Cu1—O2 | 88.07 (6) | Cu2—OW6—H62 | 124 (2) |
OW7iii—Cu1—O2 | 91.93 (6) | H61—OW6—H62 | 118 (3) |
OW8iv—Cu1—O2 | 94.72 (6) | Cu1i—OW7—H71 | 114 (2) |
OW8—Cu1—O2 | 85.28 (6) | Cu1i—OW7—H72 | 115 (2) |
O2iv—Cu1—O2 | 180.0 | H71—OW7—H72 | 109 (3) |
OW5ii—Cu2—OW5v | 180.00 (8) | Cu1—OW8—H81 | 127 (2) |
OW5ii—Cu2—OW6vi | 89.53 (7) | Cu1—OW8—H82 | 115 (3) |
OW5v—Cu2—OW6vi | 90.47 (7) | H81—OW8—H82 | 109 (3) |
OW5ii—Cu2—OW6 | 90.47 (7) | H91—OW9—H92 | 104 (3) |
OW5v—Cu2—OW6 | 89.53 (7) | | |
| | | |
OW7ii—Cu1—O2—Seiii | −86.30 (10) | O1i—Se—O3—Cu2vii | 22.53 (13) |
OW7iii—Cu1—O2—Seiii | 93.70 (10) | O2i—Se—O3—Cu2vii | 144.88 (10) |
OW8iv—Cu1—O2—Seiii | 5.15 (10) | O4—Se—O3—Cu2vii | −97.66 (12) |
OW8—Cu1—O2—Seiii | −174.85 (10) | | |
Symmetry codes: (i) x, y+1, z; (ii) −x+1, −y+1, −z+1; (iii) x, y−1, z; (iv) −x+1, −y, −z+1; (v) x, y, z−1; (vi) −x+1, −y+1, −z; (vii) x, y, z+1. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
OW5—H51···O1 | 0.73 (4) | 1.94 (4) | 2.668 (2) | 178 (4) |
OW5—H52···O4viii | 0.80 (3) | 1.91 (3) | 2.703 (2) | 167 (3) |
OW6—H61···O1ix | 0.75 (3) | 1.95 (3) | 2.695 (2) | 175 (3) |
OW6—H62···O4ix | 0.79 (3) | 1.98 (3) | 2.762 (2) | 169 (3) |
OW7—H71···OW9 | 0.83 (3) | 1.95 (3) | 2.772 (2) | 172 (3) |
OW7—H72···O4x | 0.80 (3) | 2.05 (3) | 2.836 (2) | 169 (3) |
OW8—H81···OW9ix | 1.04 (4) | 1.75 (4) | 2.777 (2) | 167 (4) |
OW8—H82···O3ii | 0.69 (3) | 2.16 (3) | 2.814 (2) | 159 (3) |
OW9—H91···O3 | 0.75 (3) | 2.28 (3) | 3.003 (2) | 162 (3) |
OW9—H92···O2 | 0.82 (4) | 1.97 (4) | 2.778 (2) | 168 (3) |
Symmetry codes: (ii) −x+1, −y+1, −z+1; (viii) x+1, y−1, z; (ix) −x, −y+1, −z+1; (x) −x, −y+2, −z+1. |