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The structure of copper(II) hydrogenphosphite dihydrate, CuHPO3·2H2O, has been redetermined on the basis of area-detector data. The results confirm the literature data of Handlovic [Acta Cryst. (1969), B25, 227-231] but with s.u. values about ten times lower and with all H-atom positions located. The microporous framework topology of the structure is discussed.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536802003574/mg6003sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536802003574/mg6003Isup2.hkl
Contains datablock I

Key indicators

  • Single-crystal X-ray study
  • T = 193 K
  • Mean [sigma](P-O) = 0.001 Å
  • R factor = 0.022
  • wR factor = 0.047
  • Data-to-parameter ratio = 21.4

checkCIF results

No syntax errors found

ADDSYM reports no extra symmetry


Amber Alert Alert Level B:
ABSTM_02 Alert B The ratio of expected to reported Tmax/Tmin(RR') is < 0.75 Tmin and Tmax reported: 0.406 0.710 Tmin' and Tmax expected: 0.653 0.771 RR' = 0.675 Please check that your absorption correction is appropriate.
Yellow Alert Alert Level C:
PLAT_420 Alert C D-H Without Acceptor P - H(1) ? 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 1.085 Tmax scaled 0.771 Tmin scaled 0.441 REFLT_03 From the CIF: _diffrn_reflns_theta_max 33.98 From the CIF: _reflns_number_total 1798 Count of symmetry unique reflns 1063 Completeness (_total/calc) 169.14% TEST3: Check Friedels for noncentro structure Estimate of Friedel pairs measured 735 Fraction of Friedel pairs measured 0.691 Are heavy atom types Z>Si present yes Please check that the estimate of the number of Friedel pairs is correct. If it is not, please give the correct count in the _publ_section_exptl_refinement section of the submitted CIF.
0 Alert Level A = Potentially serious problem
1 Alert Level B = Potential problem
1 Alert Level C = Please check

Computing details top

Data collection: X-AREA (Stoe & Cie, 2001); cell refinement: X-AREA; data reduction: X-AREA; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: DIAMOND (Brandenburg, 1999).

(I) top
Crystal data top
CuHPO3·2H2ODx = 2.700 Mg m3
Mr = 179.55Mo Kα radiation, λ = 0.71073 Å
Orthorhombic, P212121Cell parameters from 8000 reflections
a = 6.6906 (5) Åθ = 3.6–32.8°
b = 7.3727 (5) ŵ = 5.21 mm1
c = 8.9552 (5) ÅT = 193 K
V = 441.74 (5) Å3Block, light blue
Z = 40.08 × 0.06 × 0.05 mm
F(000) = 356
Data collection top
Stoe IPDS-II image-plate
diffractometer
1798 independent reflections
Radiation source: fine-focus sealed tube1765 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.087
D=90 mm, Δω = 1°, 5 min/rec scansθmax = 34.0°, θmin = 3.6°
Absorption correction: multi-scan
(SHELXTL; Sheldrick, 1996)
h = 1010
Tmin = 0.406, Tmax = 0.710k = 1111
11632 measured reflectionsl = 1414
Refinement top
Refinement on F2Hydrogen site location: difference Fourier map
Least-squares matrix: fullAll H-atom parameters refined
R[F2 > 2σ(F2)] = 0.022 w = 1/[σ2(Fo2) + (0.02P)2 + 0.05P]
where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.047(Δ/σ)max < 0.001
S = 1.10Δρmax = 0.66 e Å3
1798 reflectionsΔρmin = 0.62 e Å3
84 parametersExtinction correction: SHELXL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
0 restraintsExtinction coefficient: 0.019 (3)
Primary atom site location: structure-invariant direct methodsAbsolute structure: Flack (1983)
Secondary atom site location: difference Fourier mapAbsolute structure parameter: 0.010 (8)
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
Cu0.26767 (2)0.02867 (2)0.095756 (17)0.00937 (6)
P0.01075 (5)0.31863 (5)0.14769 (4)0.00821 (7)
O10.02312 (17)0.38942 (15)0.30688 (11)0.01191 (18)
O20.21498 (17)0.22526 (14)0.14162 (12)0.01153 (17)
O30.00358 (16)0.47100 (16)0.03114 (11)0.01178 (16)
O40.29938 (18)0.28458 (16)0.03218 (12)0.0144 (2)
H410.184 (5)0.350 (5)0.033 (4)0.031 (6)*
H420.353 (5)0.304 (5)0.054 (4)0.031 (6)*
O50.45467 (19)0.05250 (18)0.31261 (14)0.0181 (2)
H510.512 (5)0.042 (5)0.324 (3)0.021 (4)*
H520.549 (5)0.123 (4)0.325 (3)0.021 (4)*
H10.113 (4)0.208 (3)0.119 (3)0.008 (5)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Cu0.01033 (8)0.00762 (8)0.01016 (8)0.00021 (5)0.00246 (5)0.00008 (5)
P0.00875 (14)0.00723 (13)0.00863 (13)0.0002 (1)0.0000 (1)0.0002 (2)
O10.0116 (4)0.0139 (4)0.0102 (4)0.0028 (4)0.0016 (3)0.0008 (3)
O20.0114 (4)0.0094 (4)0.0137 (4)0.0020 (4)0.0002 (3)0.0007 (3)
O30.0123 (4)0.0106 (3)0.0124 (4)0.0006 (4)0.0028 (3)0.0027 (4)
O40.0162 (5)0.0105 (4)0.0166 (4)0.0023 (4)0.0051 (4)0.0023 (4)
O50.0161 (5)0.0167 (5)0.0217 (5)0.0009 (4)0.0053 (4)0.0010 (4)
Geometric parameters (Å, º) top
Cu—O21.9488 (10)P—O31.5364 (11)
Cu—O1i1.9499 (11)P—H11.19 (2)
Cu—O3ii1.9531 (10)O1—Cuiv1.9499 (11)
Cu—O41.9822 (12)O3—Cuv1.9531 (10)
Cu—O52.3168 (12)O4—H410.91 (3)
Cu—O5iii3.0001 (13)O4—H420.86 (4)
P—O21.5310 (12)O5—H510.80 (3)
P—O11.5349 (11)O5—H520.82 (3)
O2—Cu—O1i92.95 (5)O2—P—O1108.52 (6)
O2—Cu—O3ii93.17 (5)O2—P—O3111.12 (6)
O1i—Cu—O3ii170.12 (4)O1—P—O3111.91 (6)
O2—Cu—O4173.88 (5)O2—P—H1107.8 (12)
O1i—Cu—O485.61 (5)O1—P—H1109.1 (12)
O3ii—Cu—O487.49 (5)O3—P—H1108.3 (12)
O2—Cu—O589.65 (5)P—O1—Cuiv130.13 (7)
O1i—Cu—O593.14 (5)P—O2—Cu126.93 (7)
O3ii—Cu—O594.65 (5)P—O3—Cuv127.11 (7)
O4—Cu—O596.36 (5)Cu—O4—H41114 (2)
O2—Cu—O5iii84.08 (4)Cu—O4—H42117 (2)
O1i—Cu—O5iii91.36 (4)H41—O4—H42106 (3)
O3ii—Cu—O5iii81.57 (4)Cu—O5—H51108 (2)
O4—Cu—O5iii90.01 (4)Cu—O5—H52125 (2)
O5—Cu—O5iii172.461 (11)H51—O5—H52100 (3)
Symmetry codes: (i) x, y+1/2, z+1/2; (ii) x+1/2, y1/2, z; (iii) x+1/2, y, z1/2; (iv) x, y1/2, z+1/2; (v) x1/2, y1/2, z.
 

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