research papers
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
Crystallographic Information File (CIF) https://doi.org/10.1107/S0108768105028387/bs5017sup1.cif | |
Rietveld powder data file (CIF format) https://doi.org/10.1107/S0108768105028387/bs5017sup2.rtv | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108768105028387/bs5017sup3.hkl |
CCDC reference: 292323
(CD_PAPER_2_publ) top
Crystal data top
C6Cd3O12P2 | V = 698.89 (4) Å3 |
Mr = 663.23 | Z = 2 |
Monoclinic, P21 | Kα1, Kα2 radiation, λ = 1.540500, 1.544300 Å |
a = 8.7743 (3) Å | T = 296 K |
b = 9.4828 (3) Å | ?, ? × ? × ? mm |
c = 9.1670 (3) Å | Specimen preparation: Prepared at 296 K |
β = 113.609 (2)° |
Refinement top
Least-squares matrix: full | Profile 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 = 0.075 | 91 parameters |
Rwp = 0.102 | 54 restraints |
Rexp = 0.060 | (Δ/σ)max = 5.46 |
R(F2) = 0.07267 | Background 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 = 3.572 | Preferred 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
C6Cd3O12P2 | β = 113.609 (2)° |
Mr = 663.23 | V = 698.89 (4) Å3 |
Monoclinic, P21 | Z = 2 |
a = 8.7743 (3) Å | Kα1, Kα2 radiation, λ = 1.540500, 1.544300 Å |
b = 9.4828 (3) Å | T = 296 K |
c = 9.1670 (3) Å | ?, ? × ? × ? mm |
Refinement top
Rp = 0.075 | ? data points |
Rwp = 0.102 | 91 parameters |
Rexp = 0.060 | 54 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
x | y | z | Uiso*/Ueq | ||
CD1 | 0.5120 (9) | 0.192 (3) | 0.7580 (8) | 0.0267 (5)* | |
CD2 | 0.5892 (6) | 0.0719 (6) | 0.3573 (6) | 0.0267 (5)* | |
CD3 | 0.3921 (6) | 0.3397 (7) | 0.1163 (6) | 0.0267 (5)* | |
P1 | 0.652 (2) | 0.4047 (14) | 0.517 (2) | 0.027 (4)* | |
P2 | 0.603 (2) | 0.4950 (14) | 0.011 (3) | 0.027 (4)* | |
O1 | 0.462 (4) | 0.8717 (18) | 0.398 (4) | 0.036 (3)* | |
O2 | 0.611 (4) | 0.4997 (17) | 0.180 (4) | 0.036 (3)* | |
O3 | 0.601 (4) | 0.3140 (17) | 0.368 (5) | 0.036 (3)* | |
O4 | 0.485 (4) | 0.1234 (17) | 0.083 (4) | 0.036 (3)* | |
O5 | 0.269 (5) | 0.5360 (18) | 0.170 (5) | 0.036 (3)* | |
O6 | 0.111 (4) | 0.3570 (17) | 0.049 (4) | 0.036 (3)* | |
O7 | 0.632 (4) | 0.5606 (18) | 0.465 (4) | 0.036 (3)* | |
O8 | 0.763 (4) | 0.1306 (17) | 0.233 (4) | 0.036 (3)* | |
O9 | 0.695 (5) | 0.8568 (17) | 0.325 (4) | 0.036 (3)* | |
C1 | 0.132 (7) | 0.8789 (19) | 0.361 (6) | 0.043 (10)* | |
C2 | 0.811 (7) | 0.4849 (18) | 0.020 (6) | 0.043 (10)* | |
C3 | −0.006 (6) | 0.9902 (19) | 0.276 (7) | 0.043 (10)* | |
C4 | 0.986 (6) | 0.5558 (19) | 0.088 (6) | 0.043 (10)* | |
C5 | 0.130 (6) | 0.4987 (19) | 0.050 (7) | 0.043 (10)* | |
C6 | 0.917 (6) | 0.1378 (19) | 0.225 (7) | 0.043 (10)* | |
O10 | 0.492 (4) | 0.8625 (17) | 0.068 (4) | 0.036 (3)* | |
O11 | 0.167 (4) | 0.5696 (17) | 0.417 (4) | 0.036 (3)* | |
O12 | 0.010 (4) | 0.2249 (18) | 0.346 (4) | 0.036 (3)* |
Geometric parameters (Å, º) top
CD1—CD3i | 3.53 (3) | O2—CD1iv | 2.30 (4) |
CD1—O1i | 2.30 (4) | O2—CD3 | 2.33 (3) |
CD1—O2i | 2.30 (4) | O2—P2 | 1.52 (4) |
CD1—O5i | 2.31 (4) | O3—CD2 | 2.298 (18) |
CD1—O7i | 2.29 (3) | O3—CD3 | 2.31 (4) |
CD1—O9i | 2.28 (4) | O3—P1 | 1.52 (4) |
CD1—O10i | 2.28 (4) | O4—CD2 | 2.36 (3) |
CD2—CD3 | 3.356 (6) | O4—CD3 | 2.27 (2) |
CD2—P1i | 3.20 (2) | O4—P2ii | 1.52 (3) |
CD2—P2ii | 3.20 (2) | O5—CD1iv | 2.31 (4) |
CD2—O1iii | 2.31 (3) | O5—CD3 | 2.31 (3) |
CD2—O3 | 2.298 (18) | O5—C5 | 1.32 (6) |
CD2—O4 | 2.36 (3) | O6—CD3 | 2.30 (3) |
CD2—O8 | 2.31 (4) | O6—C5 | 1.35 (3) |
CD2—O9iii | 2.31 (2) | O7—CD1iv | 2.29 (3) |
CD2—O11i | 2.31 (3) | O7—P1 | 1.54 (2) |
CD3—CD1iv | 3.53 (3) | O8—CD2 | 2.31 (4) |
CD3—CD2 | 3.356 (6) | O8—C6 | 1.38 (6) |
CD3—P2 | 2.82 (2) | O9—CD1iv | 2.28 (4) |
CD3—O2 | 2.33 (3) | O9—CD2vi | 2.31 (2) |
CD3—O3 | 2.31 (4) | C1—P1iv | 1.79 (5) |
CD3—O4 | 2.27 (2) | C1—C3 | 1.56 (5) |
CD3—O5 | 2.31 (3) | C2—P2 | 1.80 (6) |
CD3—O6 | 2.30 (3) | C2—C4 | 1.56 (6) |
CD3—C5 | 2.61 (4) | C3—C1 | 1.56 (5) |
CD3—O10ii | 2.31 (4) | C3—C6vii | 1.54 (4) |
P1—CD2iv | 3.20 (2) | C4—C2 | 1.56 (6) |
P1—O1i | 1.52 (4) | C4—C5viii | 1.54 (7) |
P1—O3 | 1.52 (4) | C5—CD3 | 2.61 (4) |
P1—O7 | 1.54 (2) | C5—O5 | 1.32 (6) |
P1—C1i | 1.79 (5) | C5—O6 | 1.35 (3) |
P2—CD2v | 3.20 (2) | C5—C4ix | 1.54 (7) |
P2—CD3 | 2.82 (2) | C6—O8 | 1.38 (6) |
P2—O2 | 1.52 (4) | C6—C3x | 1.54 (4) |
P2—O4v | 1.52 (3) | C6—O12viii | 1.36 (4) |
P2—C2 | 1.80 (6) | O10—CD1iv | 2.28 (4) |
P2—O10ii | 1.52 (3) | O10—CD3v | 2.31 (4) |
O1—CD1iv | 2.30 (4) | O10—P2v | 1.52 (3) |
O1—CD2vi | 2.31 (3) | O11—CD2iv | 2.31 (3) |
O1—P1iv | 1.52 (4) | O12—C6ix | 1.36 (4) |
O1i—CD1—O2i | 156.4 (13) | O6—CD3—O10ii | 122.6 (12) |
O1i—CD1—O5i | 111.9 (13) | O1i—P1—O3 | 108.8 (19) |
O1i—CD1—O7i | 90.2 (10) | O1i—P1—O7 | 110 (2) |
O1i—CD1—O9i | 63.4 (14) | O1i—P1—C1i | 114 (2) |
O1i—CD1—O10i | 86.8 (15) | O3—P1—O7 | 107.9 (19) |
O2i—CD1—O5i | 80.8 (15) | O3—P1—C1i | 110 (2) |
O2i—CD1—O7i | 69.2 (14) | O7—P1—C1i | 106.6 (16) |
O2i—CD1—O9i | 103.5 (11) | CD3—P2—O2 | 55.8 (12) |
O2i—CD1—O10i | 104.4 (12) | CD3—P2—O4v | 111.1 (16) |
O5i—CD1—O7i | 90.2 (14) | CD3—P2—C2 | 138.7 (12) |
O5i—CD1—O9i | 175.3 (18) | CD3—P2—O10ii | 54.9 (17) |
O5i—CD1—O10i | 120.1 (11) | O2—P2—O4v | 111.2 (19) |
O7i—CD1—O9i | 89.7 (10) | O2—P2—C2 | 109 (2) |
O7i—CD1—O10i | 148.4 (12) | O2—P2—O10ii | 108 (2) |
O9i—CD1—O10i | 60.9 (12) | O4v—P2—C2 | 110 (2) |
O1iii—CD2—O3 | 146.1 (14) | O4v—P2—O10ii | 109.5 (18) |
O1iii—CD2—O4 | 109.8 (10) | C2—P2—O10ii | 109.1 (19) |
O1iii—CD2—O8 | 137.6 (10) | CD1iv—O1—CD2vi | 109.3 (18) |
O1iii—CD2—O9iii | 62.8 (12) | CD1iv—O1—P1iv | 136.1 (17) |
O1iii—CD2—O11i | 100.5 (10) | CD2vi—O1—P1iv | 112.0 (12) |
O3—CD2—O4 | 80.2 (11) | CD1iv—O2—CD3 | 99.0 (15) |
O3—CD2—O8 | 75.7 (12) | CD1iv—O2—P2 | 116.2 (15) |
O3—CD2—O9iii | 150.9 (14) | CD3—O2—P2 | 91.7 (15) |
O3—CD2—O11i | 87.8 (10) | CD2—O3—CD3 | 93.3 (11) |
O4—CD2—O8 | 58.2 (11) | CD2—O3—P1 | 127 (2) |
O4—CD2—O9iii | 92.8 (10) | CD3—O3—P1 | 131.9 (16) |
O4—CD2—O11i | 141.4 (11) | CD2—O4—CD3 | 92.9 (11) |
O8—CD2—O9iii | 76.6 (11) | CD2—O4—P2ii | 109.5 (15) |
O8—CD2—O11i | 83.3 (11) | CD3—O4—P2ii | 132.3 (19) |
O9iii—CD2—O11i | 80.2 (10) | CD1iv—O5—CD3 | 99.7 (16) |
P2—CD3—O2 | 32.5 (10) | CD1iv—O5—C5 | 143 (3) |
P2—CD3—O3 | 91.8 (10) | CD3—O5—C5 | 88 (2) |
P2—CD3—O4 | 96.0 (9) | CD3—O6—C5 | 87 (3) |
P2—CD3—O5 | 94.6 (10) | CD1iv—O7—P1 | 138.7 (18) |
P2—CD3—O6 | 130.7 (8) | CD2—O8—C6 | 153 (3) |
P2—CD3—O10ii | 32.6 (7) | CD1iv—O9—CD2vi | 109.7 (17) |
O2—CD3—O3 | 65.0 (11) | P1iv—C1—C3 | 130 (2) |
O2—CD3—O4 | 108.4 (11) | P2—C2—C4 | 145 (3) |
O2—CD3—O5 | 80.3 (11) | C1—C3—C6vii | 157 (4) |
O2—CD3—O6 | 135.1 (8) | C2—C4—C5viii | 122 (3) |
O2—CD3—O10ii | 63.9 (12) | O5—C5—O6 | 110 (3) |
O3—CD3—O4 | 81.7 (10) | O5—C5—C4ix | 106 (5) |
O3—CD3—O5 | 97.0 (12) | O6—C5—C4ix | 104 (4) |
O3—CD3—O6 | 127.6 (14) | O8—C6—C3x | 105 (4) |
O3—CD3—O10ii | 109.6 (13) | O8—C6—O12viii | 105 (5) |
O4—CD3—O5 | 169.3 (12) | C3x—C6—O12viii | 105 (4) |
O4—CD3—O6 | 115.7 (9) | CD1iv—O10—CD3v | 125.5 (11) |
O4—CD3—O10ii | 72.4 (10) | CD1iv—O10—P2v | 140 (3) |
O5—CD3—O6 | 56.8 (10) | CD3v—O10—P2v | 93 (2) |
O5—CD3—O10ii | 117.7 (11) |
Symmetry codes: (i) −x+1, y−1/2, −z+1; (ii) −x+1, y−1/2, −z; (iii) x, y−1, z; (iv) −x+1, y+1/2, −z+1; (v) −x+1, y+1/2, −z; (vi) x, y+1, z; (vii) x−1, y+1, z; (viii) x+1, y, z; (ix) x−1, y, z; (x) x+1, y−1, z. |
Experimental details
Crystal data | |
Chemical formula | C6Cd3O12P2 |
Mr | 663.23 |
Crystal system, space group | Monoclinic, P21 |
Temperature (K) | 296 |
a, b, c (Å) | 8.7743 (3), 9.4828 (3), 9.1670 (3) |
β (°) | 113.609 (2) |
V (Å3) | 698.89 (4) |
Z | 2 |
Radiation type | Kα1, Kα2, λ = 1.540500, 1.544300 Å |
Specimen shape, size (mm) | ?, ? × ? × ? |
Data collection | |
Diffractometer | ? |
Specimen mounting | ? |
Data collection mode | ? |
Scan method | Step |
2θ values (°) | 2θmin = ? 2θmax = ? 2θstep = ? |
Refinement | |
R factors and goodness of fit | Rp = 0.075, Rwp = 0.102, Rexp = 0.060, R(F2) = 0.07267, χ2 = 3.572 |
No. of data points | ? |
No. of parameters | 91 |
No. of restraints | 54 |
(Δ/σ)max | 5.46 |
Computer programs: GSAS.