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The title compound poly[[bis(μ-2-carboxylatoethylphosphonato)cadmium] dihydrate], Cd3(O3PC2H4CO2)2·2H2O, was prepared by a hydrothermal reaction and its crystal structure determined from in-house powder data. The structure was solved in both P21/c and P21 space groups. The refinement converged with Rp = 0.1046, Rwp = 0.1378 and Rf = 0.0763 in P21/c. However, the solid-state NMR data could not be explained. The structure was then solved in P21 and the refinement converged with Rp = 0.0750, Rwp = 0.1022 and Rf = 0.0409 and satisfied the NMR requirements.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108768105028387/bs5017sup1.cif
Contains datablock CD_PAPER_2_publ

rtv

Rietveld powder data file (CIF format) https://doi.org/10.1107/S0108768105028387/bs5017sup2.rtv
Supplementary material

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108768105028387/bs5017sup3.hkl
Supplementary material

CCDC reference: 292323

Computing details top

Program(s) used to refine structure: GSAS.

Figures top
[Figure 1]
[Figure 2]
[Figure 3]
[Figure 4]
[Figure 5]
[Figure 6]
[Figure 7]
(CD_PAPER_2_publ) top
Crystal data top
C6Cd3O12P2V = 698.89 (4) Å3
Mr = 663.23Z = 2
Monoclinic, P21 Kα1, Kα2 radiation, λ = 1.540500, 1.544300 Å
a = 8.7743 (3) ÅT = 296 K
b = 9.4828 (3) Å?, ? × ? × ? mm
c = 9.1670 (3) ÅSpecimen preparation: Prepared at 296 K
β = 113.609 (2)°
Data collection top
Scan method: step
Refinement top
Least-squares matrix: fullProfile function: CW Profile function number 4 with 21 terms Pseudovoigt profile coefficients as parameterized in P. Thompson, D.E. Cox & J.B. Hastings (1987). J. Appl. Cryst.,20,79-83. Asymmetry correction of L.W. Finger, D.E. Cox & A. P. Jephcoat (1994). J. Appl. Cryst.,27,892-900. Microstrain broadening by P.W. Stephens, (1999). J. Appl. Cryst.,32,281-289. #1(GU) = 64.419 #2(GV) = -24.294 #3(GW) = 5.301 #4(GP) = 0.331 #5(LX) = 0.000 #6(ptec) = 0.00 #7(trns) = 8.70 #8(shft) = 0.0000 #9(sfec) = 0.00 #10(S/L) = 0.0285 #11(H/L) = 0.0248 #12(eta) = 0.9820 #13(S400 ) = 2.1E-01 #14(S040 ) = 8.4E-02 #15(S004 ) = 2.7E-01 #16(S220 ) = 8.3E-02 #17(S202 ) = 3.7E-01 #18(S022 ) = 1.1E-01 #19(S301 ) = 1.7E-01 #20(S103 ) = 3.7E-01 #21(S121 ) = 3.9E-02 Peak tails are ignored where the intensity is below 0.0100 times the peak Aniso. broadening axis 0.0 0.0 1.0
Rp = 0.07591 parameters
Rwp = 0.10254 restraints
Rexp = 0.060(Δ/σ)max = 5.46
R(F2) = 0.07267Background function: GSAS Background function number 1 with 4 terms. Shifted Chebyshev function of 1st kind 1: 81.6696 2: -39.5945 3: 6.98397 4: -11.7786
χ2 = 3.572Preferred orientation correction: March-Dollase AXIS 1 Ratio= 0.695 Frac 0.062 h= 1.000 k= 0.000 l= 0.000 AXIS 2 Ratio= 0.936 Frac 0.938 h= 1.000 k= 1.000 l= 1.000
**** Spherical Harmonic ODF **** Spherical harmonic order= 16 The sample symmetry is: cylindrical (fiber texture) Index = 2 0 -2 Coeff= 0.1237 Index = 2 0 0 Coeff= -0.1480 Index = 2 0 2 Coeff= -0.0529 Index = 4 0 -4 Coeff= -0.0230 Index = 4 0 -2 Coeff= 0.4076 Index = 4 0 0 Coeff= 0.3639 Index = 4 0 2 Coeff= -0.1568 Index = 4 0 4 Coeff= 0.2879 Index = 6 0 -6 Coeff= -0.3768 Index = 6 0 -4 Coeff= -0.0598 Index = 6 0 -2 Coeff= -0.2882 Index = 6 0 0 Coeff= 1.2562 Index = 6 0 2 Coeff= -0.3678 Index = 6 0 4 Coeff= -0.2825 Index = 6 0 6 Coeff= -0.1684 Index = 8 0 -8 Coeff= -0.2025 Index = 8 0 -6 Coeff= -0.4956 Index = 8 0 -4 Coeff= -0.6262 Index = 8 0 -2 Coeff= -0.6775 Index = 8 0 0 Coeff= -0.3945 Index = 8 0 2 Coeff= -0.5905 Index = 8 0 4 Coeff= -0.3387 Index = 8 0 6 Coeff= -0.1318 Index = 8 0 8 Coeff= -0.3786 Index = 10 0-10 Coeff= 0.0323 Index = 10 0 -8 Coeff= -0.0574 Index = 10 0 -6 Coeff= -0.7677 Index = 10 0 -4 Coeff= -0.1146 Index = 10 0 -2 Coeff= -0.2396 Index = 10 0 0 Coeff= 0.7262 Index = 10 0 2 Coeff= 0.0330 Index = 10 0 4 Coeff= 0.3847 Index = 10 0 6 Coeff= 1.2708 Index = 10 0 8 Coeff= 0.4336 Index = 10 0 10 Coeff= 0.1258 Index = 12 0-12 Coeff= 0.3298 Index = 12 0-10 Coeff= 0.2353 Index = 12 0 -8 Coeff= -0.2870 Index = 12 0 -6 Coeff= 0.1873 Index = 12 0 -4 Coeff= -0.4632 Index = 12 0 -2 Coeff= 0.2010 Index = 12 0 0 Coeff= -0.3965 Index = 12 0 2 Coeff= 0.1869 Index = 12 0 4 Coeff= -0.1183 Index = 12 0 6 Coeff= -0.0995 Index = 12 0 8 Coeff= -0.6403 Index = 12 0 10 Coeff= 0.0964 Index = 12 0 12 Coeff= 0.0407 Index = 14 0-14 Coeff= -0.0938 Index = 14 0-12 Coeff= -0.3328 Index = 14 0-10 Coeff= -0.5294 Index = 14 0 -8 Coeff= -0.5834 Index = 14 0 -6 Coeff= 0.1683 Index = 14 0 -4 Coeff= 0.0067 Index = 14 0 -2 Coeff= 0.4727 Index = 14 0 0 Coeff= 0.4474 Index = 14 0 2 Coeff= -0.4905 Index = 14 0 4 Coeff= 0.7846 Index = 14 0 6 Coeff= 0.6738 Index = 14 0 8 Coeff= -0.4932 Index = 14 0 10 Coeff= -0.6313 Index = 14 0 12 Coeff= -0.1521 Index = 14 0 14 Coeff= 0.2573 Index = 16 0-16 Coeff= -0.1691 Index = 16 0-14 Coeff= -0.3010 Index = 16 0-12 Coeff= 0.2995 Index = 16 0-10 Coeff= -0.3543 Index = 16 0 -8 Coeff= 0.4720 Index = 16 0 -6 Coeff= -0.0406 Index = 16 0 -4 Coeff= -0.6123 Index = 16 0 -2 Coeff= -0.3133 Index = 16 0 0 Coeff= 0.3555 Index = 16 0 2 Coeff= -0.1515 Index = 16 0 4 Coeff= 0.4395 Index = 16 0 6 Coeff= -0.1596 Index = 16 0 8 Coeff= 0.3169 Index = 16 0 10 Coeff= 0.2061 Index = 16 0 12 Coeff= 0.1799 Index = 16 0 14 Coeff= 0.2010 Index = 16 0 16 Coeff= 0.0583 Prefered orientation correction range: Min= 0.25463, Max= 1.95348
? data points
Crystal data top
C6Cd3O12P2β = 113.609 (2)°
Mr = 663.23V = 698.89 (4) Å3
Monoclinic, P21Z = 2
a = 8.7743 (3) Å Kα1, Kα2 radiation, λ = 1.540500, 1.544300 Å
b = 9.4828 (3) ÅT = 296 K
c = 9.1670 (3) Å?, ? × ? × ? mm
Data collection top
Scan method: step
Refinement top
Rp = 0.075? data points
Rwp = 0.10291 parameters
Rexp = 0.06054 restraints
R(F2) = 0.07267(Δ/σ)max = 5.46
χ2 = 3.572
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
CD10.5120 (9)0.192 (3)0.7580 (8)0.0267 (5)*
CD20.5892 (6)0.0719 (6)0.3573 (6)0.0267 (5)*
CD30.3921 (6)0.3397 (7)0.1163 (6)0.0267 (5)*
P10.652 (2)0.4047 (14)0.517 (2)0.027 (4)*
P20.603 (2)0.4950 (14)0.011 (3)0.027 (4)*
O10.462 (4)0.8717 (18)0.398 (4)0.036 (3)*
O20.611 (4)0.4997 (17)0.180 (4)0.036 (3)*
O30.601 (4)0.3140 (17)0.368 (5)0.036 (3)*
O40.485 (4)0.1234 (17)0.083 (4)0.036 (3)*
O50.269 (5)0.5360 (18)0.170 (5)0.036 (3)*
O60.111 (4)0.3570 (17)0.049 (4)0.036 (3)*
O70.632 (4)0.5606 (18)0.465 (4)0.036 (3)*
O80.763 (4)0.1306 (17)0.233 (4)0.036 (3)*
O90.695 (5)0.8568 (17)0.325 (4)0.036 (3)*
C10.132 (7)0.8789 (19)0.361 (6)0.043 (10)*
C20.811 (7)0.4849 (18)0.020 (6)0.043 (10)*
C30.006 (6)0.9902 (19)0.276 (7)0.043 (10)*
C40.986 (6)0.5558 (19)0.088 (6)0.043 (10)*
C50.130 (6)0.4987 (19)0.050 (7)0.043 (10)*
C60.917 (6)0.1378 (19)0.225 (7)0.043 (10)*
O100.492 (4)0.8625 (17)0.068 (4)0.036 (3)*
O110.167 (4)0.5696 (17)0.417 (4)0.036 (3)*
O120.010 (4)0.2249 (18)0.346 (4)0.036 (3)*
Geometric parameters (Å, º) top
CD1—CD3i3.53 (3)O2—CD1iv2.30 (4)
CD1—O1i2.30 (4)O2—CD32.33 (3)
CD1—O2i2.30 (4)O2—P21.52 (4)
CD1—O5i2.31 (4)O3—CD22.298 (18)
CD1—O7i2.29 (3)O3—CD32.31 (4)
CD1—O9i2.28 (4)O3—P11.52 (4)
CD1—O10i2.28 (4)O4—CD22.36 (3)
CD2—CD33.356 (6)O4—CD32.27 (2)
CD2—P1i3.20 (2)O4—P2ii1.52 (3)
CD2—P2ii3.20 (2)O5—CD1iv2.31 (4)
CD2—O1iii2.31 (3)O5—CD32.31 (3)
CD2—O32.298 (18)O5—C51.32 (6)
CD2—O42.36 (3)O6—CD32.30 (3)
CD2—O82.31 (4)O6—C51.35 (3)
CD2—O9iii2.31 (2)O7—CD1iv2.29 (3)
CD2—O11i2.31 (3)O7—P11.54 (2)
CD3—CD1iv3.53 (3)O8—CD22.31 (4)
CD3—CD23.356 (6)O8—C61.38 (6)
CD3—P22.82 (2)O9—CD1iv2.28 (4)
CD3—O22.33 (3)O9—CD2vi2.31 (2)
CD3—O32.31 (4)C1—P1iv1.79 (5)
CD3—O42.27 (2)C1—C31.56 (5)
CD3—O52.31 (3)C2—P21.80 (6)
CD3—O62.30 (3)C2—C41.56 (6)
CD3—C52.61 (4)C3—C11.56 (5)
CD3—O10ii2.31 (4)C3—C6vii1.54 (4)
P1—CD2iv3.20 (2)C4—C21.56 (6)
P1—O1i1.52 (4)C4—C5viii1.54 (7)
P1—O31.52 (4)C5—CD32.61 (4)
P1—O71.54 (2)C5—O51.32 (6)
P1—C1i1.79 (5)C5—O61.35 (3)
P2—CD2v3.20 (2)C5—C4ix1.54 (7)
P2—CD32.82 (2)C6—O81.38 (6)
P2—O21.52 (4)C6—C3x1.54 (4)
P2—O4v1.52 (3)C6—O12viii1.36 (4)
P2—C21.80 (6)O10—CD1iv2.28 (4)
P2—O10ii1.52 (3)O10—CD3v2.31 (4)
O1—CD1iv2.30 (4)O10—P2v1.52 (3)
O1—CD2vi2.31 (3)O11—CD2iv2.31 (3)
O1—P1iv1.52 (4)O12—C6ix1.36 (4)
O1i—CD1—O2i156.4 (13)O6—CD3—O10ii122.6 (12)
O1i—CD1—O5i111.9 (13)O1i—P1—O3108.8 (19)
O1i—CD1—O7i90.2 (10)O1i—P1—O7110 (2)
O1i—CD1—O9i63.4 (14)O1i—P1—C1i114 (2)
O1i—CD1—O10i86.8 (15)O3—P1—O7107.9 (19)
O2i—CD1—O5i80.8 (15)O3—P1—C1i110 (2)
O2i—CD1—O7i69.2 (14)O7—P1—C1i106.6 (16)
O2i—CD1—O9i103.5 (11)CD3—P2—O255.8 (12)
O2i—CD1—O10i104.4 (12)CD3—P2—O4v111.1 (16)
O5i—CD1—O7i90.2 (14)CD3—P2—C2138.7 (12)
O5i—CD1—O9i175.3 (18)CD3—P2—O10ii54.9 (17)
O5i—CD1—O10i120.1 (11)O2—P2—O4v111.2 (19)
O7i—CD1—O9i89.7 (10)O2—P2—C2109 (2)
O7i—CD1—O10i148.4 (12)O2—P2—O10ii108 (2)
O9i—CD1—O10i60.9 (12)O4v—P2—C2110 (2)
O1iii—CD2—O3146.1 (14)O4v—P2—O10ii109.5 (18)
O1iii—CD2—O4109.8 (10)C2—P2—O10ii109.1 (19)
O1iii—CD2—O8137.6 (10)CD1iv—O1—CD2vi109.3 (18)
O1iii—CD2—O9iii62.8 (12)CD1iv—O1—P1iv136.1 (17)
O1iii—CD2—O11i100.5 (10)CD2vi—O1—P1iv112.0 (12)
O3—CD2—O480.2 (11)CD1iv—O2—CD399.0 (15)
O3—CD2—O875.7 (12)CD1iv—O2—P2116.2 (15)
O3—CD2—O9iii150.9 (14)CD3—O2—P291.7 (15)
O3—CD2—O11i87.8 (10)CD2—O3—CD393.3 (11)
O4—CD2—O858.2 (11)CD2—O3—P1127 (2)
O4—CD2—O9iii92.8 (10)CD3—O3—P1131.9 (16)
O4—CD2—O11i141.4 (11)CD2—O4—CD392.9 (11)
O8—CD2—O9iii76.6 (11)CD2—O4—P2ii109.5 (15)
O8—CD2—O11i83.3 (11)CD3—O4—P2ii132.3 (19)
O9iii—CD2—O11i80.2 (10)CD1iv—O5—CD399.7 (16)
P2—CD3—O232.5 (10)CD1iv—O5—C5143 (3)
P2—CD3—O391.8 (10)CD3—O5—C588 (2)
P2—CD3—O496.0 (9)CD3—O6—C587 (3)
P2—CD3—O594.6 (10)CD1iv—O7—P1138.7 (18)
P2—CD3—O6130.7 (8)CD2—O8—C6153 (3)
P2—CD3—O10ii32.6 (7)CD1iv—O9—CD2vi109.7 (17)
O2—CD3—O365.0 (11)P1iv—C1—C3130 (2)
O2—CD3—O4108.4 (11)P2—C2—C4145 (3)
O2—CD3—O580.3 (11)C1—C3—C6vii157 (4)
O2—CD3—O6135.1 (8)C2—C4—C5viii122 (3)
O2—CD3—O10ii63.9 (12)O5—C5—O6110 (3)
O3—CD3—O481.7 (10)O5—C5—C4ix106 (5)
O3—CD3—O597.0 (12)O6—C5—C4ix104 (4)
O3—CD3—O6127.6 (14)O8—C6—C3x105 (4)
O3—CD3—O10ii109.6 (13)O8—C6—O12viii105 (5)
O4—CD3—O5169.3 (12)C3x—C6—O12viii105 (4)
O4—CD3—O6115.7 (9)CD1iv—O10—CD3v125.5 (11)
O4—CD3—O10ii72.4 (10)CD1iv—O10—P2v140 (3)
O5—CD3—O656.8 (10)CD3v—O10—P2v93 (2)
O5—CD3—O10ii117.7 (11)
Symmetry codes: (i) x+1, y1/2, z+1; (ii) x+1, y1/2, z; (iii) x, y1, z; (iv) x+1, y+1/2, z+1; (v) x+1, y+1/2, z; (vi) x, y+1, z; (vii) x1, y+1, z; (viii) x+1, y, z; (ix) x1, y, z; (x) x+1, y1, z.

Experimental details

Crystal data
Chemical formulaC6Cd3O12P2
Mr663.23
Crystal system, space groupMonoclinic, P21
Temperature (K)296
a, b, c (Å)8.7743 (3), 9.4828 (3), 9.1670 (3)
β (°) 113.609 (2)
V3)698.89 (4)
Z2
Radiation type Kα1, Kα2, λ = 1.540500, 1.544300 Å
Specimen shape, size (mm)?, ? × ? × ?
Data collection
Diffractometer?
Specimen mounting?
Data collection mode?
Scan methodStep
2θ values (°)2θmin = ? 2θmax = ? 2θstep = ?
Refinement
R factors and goodness of fitRp = 0.075, Rwp = 0.102, Rexp = 0.060, R(F2) = 0.07267, χ2 = 3.572
No. of data points?
No. of parameters91
No. of restraints54
(Δ/σ)max5.46

Computer programs: GSAS.

 

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