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Cadmium phosphite, CdHPO3, was obtained by mild hydrothermal synthesis. The construction of the three-dimensional framework structure may be viewed as an assembly of distorted CdO6 octahedra and HPO3 tetrahedra which leads to the formation of channels along [001]. The crystal structure is isotypic with CdSO3-III and is a new example of the stereochemical equivalence of the P-bonded H atom in HPO32- and the electron lone pair in XO32- oxoanions (X = SIV or SeIV).
Supporting information
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (P-O) = 0.003 Å
- R factor = 0.027
- wR factor = 0.067
- Data-to-parameter ratio = 13.9
checkCIF/PLATON results
No syntax errors found
Alert level B
PLAT430_ALERT_2_B Short Inter D...A Contact O2 .. O3 .. 2.80 Ang.
Alert level C
PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings Differ .... ?
PLAT045_ALERT_1_C Calculated and Reported Z Differ by ............ 0.11 Ratio
Alert level G
PLAT199_ALERT_1_G Check the Reported _cell_measurement_temperature 293 K
PLAT200_ALERT_1_G Check the Reported _diffrn_ambient_temperature . 293 K
0 ALERT level A = In general: serious problem
1 ALERT level B = Potentially serious problem
2 ALERT level C = Check and explain
2 ALERT level G = General alerts; check
4 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
1 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
Data collection: SMART (Bruker, 2003); cell refinement: SAINT-Plus (Bruker, 2003); data reduction: SAINT-Plus; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Bruker, 2003) and DIAMOND (Brandenburg, 2005); software used to prepare material for publication: SHELXL97.
Cadmium phosphate(III)
top
Crystal data top
CdHPO3 | Dx = 4.342 Mg m−3 |
Mr = 192.39 | Mo Kα radiation, λ = 0.71073 Å |
Hexagonal, R3 | Cell parameters from 2109 reflections |
Hall symbol: -R 3 | θ = 3.0–27.3° |
a = 13.509 (2) Å | µ = 7.73 mm−1 |
c = 8.379 (2) Å | T = 293 K |
V = 1324.3 (4) Å3 | Block, colourless |
Z = 18 | 0.20 × 0.20 × 0.18 mm |
F(000) = 1584 | |
Data collection top
Bruker SMART APEX CCD area-detector diffractometer | 660 reflections with I > 2σ(I) |
Radiation source: fine-focus sealed tube | Rint = 0.024 |
Graphite monochromator | θmax = 27.4°, θmin = 3.0° |
ω scans | h = −10→17 |
2018 measured reflections | k = −17→17 |
679 independent reflections | l = −9→10 |
Refinement top
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.027 | Hydrogen site location: difference Fourier map |
wR(F2) = 0.067 | All H-atom parameters refined |
S = 1.03 | w = 1/[σ2(Fo2) + (0.055P)2 + 5.8207P] where P = (Fo2 + 2Fc2)/3 |
679 reflections | (Δ/σ)max = 0.012 |
49 parameters | Δρmax = 0.92 e Å−3 |
0 restraints | Δρmin = −3.51 e Å−3 |
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 | |
Cd1 | 0.44451 (2) | 0.06208 (2) | 0.23950 (3) | 0.00916 (16) | |
P1 | 0.68801 (8) | 0.16748 (8) | 0.04639 (11) | 0.0072 (2) | |
O1 | 0.6343 (2) | 0.1537 (2) | 0.2114 (3) | 0.0114 (5) | |
O3 | 0.6532 (2) | 0.0525 (2) | −0.0300 (3) | 0.0131 (6) | |
O2 | 0.8174 (2) | 0.2440 (2) | 0.0533 (3) | 0.0135 (6) | |
H1 | 0.646 (5) | 0.224 (5) | −0.043 (6) | 0.016* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Cd1 | 0.00783 (19) | 0.00993 (19) | 0.0091 (2) | 0.00400 (12) | −0.00008 (8) | 0.00032 (8) |
P1 | 0.0065 (4) | 0.0077 (4) | 0.0078 (4) | 0.0039 (3) | −0.0001 (3) | −0.0001 (3) |
O1 | 0.0094 (12) | 0.0139 (13) | 0.0111 (12) | 0.0059 (11) | 0.0005 (9) | −0.0013 (10) |
O3 | 0.0154 (13) | 0.0108 (13) | 0.0128 (13) | 0.0064 (11) | −0.0026 (11) | −0.0023 (10) |
O2 | 0.0076 (13) | 0.0126 (13) | 0.0164 (13) | 0.0022 (10) | 0.0018 (10) | −0.0040 (11) |
Geometric parameters (Å, º) top
Cd1—O1 | 2.233 (3) | P1—O1 | 1.529 (3) |
Cd1—O3i | 2.275 (3) | P1—H1 | 1.38 (5) |
Cd1—O2ii | 2.322 (3) | O1—Cd1vi | 2.333 (3) |
Cd1—O3iii | 2.325 (3) | O3—Cd1i | 2.275 (3) |
Cd1—O1iv | 2.333 (3) | O3—Cd1vii | 2.324 (3) |
Cd1—O2v | 2.353 (3) | O2—Cd1viii | 2.322 (3) |
P1—O3 | 1.521 (3) | O2—Cd1ix | 2.354 (3) |
P1—O2 | 1.523 (3) | | |
| | | |
O1—Cd1—O3i | 114.21 (10) | O3—P1—O2 | 111.91 (16) |
O1—Cd1—O2ii | 98.53 (10) | O3—P1—O1 | 111.73 (16) |
O3i—Cd1—O2ii | 91.52 (10) | O2—P1—O1 | 111.22 (17) |
O1—Cd1—O3iii | 159.24 (10) | O3—P1—H1 | 109 (2) |
O3i—Cd1—O3iii | 85.76 (3) | O2—P1—H1 | 107 (2) |
O2ii—Cd1—O3iii | 74.24 (10) | O1—P1—H1 | 105 (2) |
O1—Cd1—O1iv | 83.21 (13) | P1—O1—Cd1 | 120.41 (16) |
O3i—Cd1—O1iv | 159.60 (10) | P1—O1—Cd1vi | 118.53 (15) |
O2ii—Cd1—O1iv | 96.41 (9) | Cd1—O1—Cd1vi | 109.52 (11) |
O3iii—Cd1—O1iv | 78.41 (10) | P1—O3—Cd1i | 142.90 (17) |
O1—Cd1—O2v | 91.92 (10) | P1—O3—Cd1vii | 114.33 (15) |
O3i—Cd1—O2v | 74.57 (10) | Cd1i—O3—Cd1vii | 102.68 (11) |
O2ii—Cd1—O2v | 165.19 (10) | P1—O2—Cd1viii | 126.47 (16) |
O3iii—Cd1—O2v | 99.24 (10) | P1—O2—Cd1ix | 131.89 (16) |
O1iv—Cd1—O2v | 95.21 (10) | Cd1viii—O2—Cd1ix | 100.37 (10) |
Symmetry codes: (i) −x+1, −y, −z; (ii) −y+2/3, x−y−2/3, z+1/3; (iii) x−y−1/3, x−2/3, −z+1/3; (iv) y+1/3, −x+y+2/3, −z+2/3; (v) −x+y+1, −x+1, z; (vi) x−y+1/3, x−1/3, −z+2/3; (vii) y+2/3, −x+y+1/3, −z+1/3; (viii) −x+y+4/3, −x+2/3, z−1/3; (ix) −y+1, x−y, z. |
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