Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536807020545/hb2393sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536807020545/hb2393Isup2.hkl |
CCDC reference: 648074
Key indicators
- Single-crystal X-ray study
- T = 295 K
- Mean (C-C) = 0.004 Å
- Disorder in main residue
- R factor = 0.052
- wR factor = 0.145
- Data-to-parameter ratio = 18.4
checkCIF/PLATON results
No syntax errors found
Alert level B ABSTM02_ALERT_3_B The ratio of expected to reported Tmax/Tmin(RR') is < 0.75 Tmin and Tmax reported: 0.567 0.903 Tmin(prime) and Tmax expected: 0.767 0.901 RR(prime) = 0.737 Please check that your absorption correction is appropriate. PLAT061_ALERT_3_B Tmax/Tmin Range Test RR' too Large ............. 0.73
Alert level C PLAT029_ALERT_3_C _diffrn_measured_fraction_theta_full Low ....... 0.96 PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for O1W PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for Cd1 PLAT250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor .... 2.27 PLAT250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor .... 2.15 PLAT301_ALERT_3_C Main Residue Disorder ......................... 3.00 Perc. PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 9 PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 3 C6 H9 N3
Alert level G PLAT860_ALERT_3_G Note: Number of Least-Squares Restraints ....... 6
0 ALERT level A = In general: serious problem 2 ALERT level B = Potentially serious problem 8 ALERT level C = Check and explain 1 ALERT level G = General alerts; check 0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 4 ALERT type 2 Indicator that the structure model may be wrong or deficient 5 ALERT type 3 Indicator that the structure quality may be low 2 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check
For chemically related materials arising from cadmium acetate which contain cadmium coordinated by N-donor ligands, see: Wang et al. (2004); Ye et al. (2000); Sergienko et al. (1980). For details of the preparation, see: Xue et al. (1993).
2-Amino-4,6-dimethylpyrimidine was synthesized according to a literature procedure (Xue et al., 1993). This heterocycle (0.12 g, 1 mmol) was added to an aqueous solution (20 ml) of cadmium acetate dihydrate (0.27 g, 1 mmol). The solution was filtered and then set aside for the growth of crystals. Block-shaped crystals of (I) were harvested after a week.
The cadmium atom, which lies on a twofold rotation axis, is disordered over two positions, the disorder refining to a 0.856 (2):0.144 (2) ratio. The vibration of the minor component was restrained to be nearly isotropic. The minor component is then covalently bonded to O2, and the distortion of geometry arises from the proximity of the O1 atom. The carbon- and nitrogen-bound H atoms were treated as riding; the methyl groups were rotated to fit the electron density. The H atoms of the water molecules were placed in chemically sensible positions on the basis of hydrogen bonding interactions, but they were not refined.
Cadmium acetate forms adducts with nitrogen-donor ligands and among the known crystal structures of such materials are the bis(4-aminophenyl)methane (Wang et al., 2004), 2,2'-bipyridine (Ye et al., 2000) and diethylnicotinamide (Sergienko et al., 1980) adducts.
The title compound, (I), the product of the reaction of cadmium acetate with 2-amino-4,6-pyrimidine, has the N-heterocycle engaging instead in an outer-sphere type of coordination (i.e. interacting indirectly through hydrogen bonds). Compound (I) consists of a triaquadiacetatocadmium molecule (Cd site symmetry 2) along with an uncoordinated water molecule and two N-heterocycles (Fig. 1). The cadmium atom is five-coordinate, but the geometry is distorted towards a pentagonal bipyramid owing to two long Cd···O interactions (Table 1). Hydrogen bonds link the three entities into a three-dimensional network motif (Table 2).
For chemically related materials arising from cadmium acetate which contain cadmium coordinated by N-donor ligands, see: Wang et al. (2004); Ye et al. (2000); Sergienko et al. (1980). For details of the preparation, see: Xue et al. (1993).
Data collection: SMART (Bruker, 2004); cell refinement: SAINT (Bruker, 2004); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: X-SEED (Barbour, 2001); software used to prepare material for publication: publCIF (Westrip, 2007).
[Cd(C2H3O2)2(H2O)3]·4C6H9N3·2H2O | F(000) = 848 |
Mr = 813.22 | Dx = 1.455 Mg m−3 |
Monoclinic, P2/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2yc | Cell parameters from 3660 reflections |
a = 19.287 (1) Å | θ = 2.9–27.5° |
b = 6.7697 (4) Å | µ = 0.65 mm−1 |
c = 14.2238 (4) Å | T = 295 K |
β = 91.444 (1)° | Block, colorless |
V = 1856.56 (16) Å3 | 0.40 × 0.20 × 0.16 mm |
Z = 2 |
Bruker APEX CCD diffractometer | 4386 independent reflections |
Radiation source: fine-focus sealed tube | 3794 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.053 |
φ and ω scans | θmax = 28.2°, θmin = 1.1° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −24→25 |
Tmin = 0.567, Tmax = 0.903 | k = −8→8 |
13020 measured reflections | l = −15→18 |
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)] = 0.052 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.145 | H-atom parameters constrained |
S = 1.11 | w = 1/[σ2(Fo2) + (0.0786P)2] where P = (Fo2 + 2Fc2)/3 |
4386 reflections | (Δ/σ)max = 0.001 |
238 parameters | Δρmax = 0.88 e Å−3 |
6 restraints | Δρmin = −0.62 e Å−3 |
[Cd(C2H3O2)2(H2O)3]·4C6H9N3·2H2O | V = 1856.56 (16) Å3 |
Mr = 813.22 | Z = 2 |
Monoclinic, P2/c | Mo Kα radiation |
a = 19.287 (1) Å | µ = 0.65 mm−1 |
b = 6.7697 (4) Å | T = 295 K |
c = 14.2238 (4) Å | 0.40 × 0.20 × 0.16 mm |
β = 91.444 (1)° |
Bruker APEX CCD diffractometer | 4386 independent reflections |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | 3794 reflections with I > 2σ(I) |
Tmin = 0.567, Tmax = 0.903 | Rint = 0.053 |
13020 measured reflections |
R[F2 > 2σ(F2)] = 0.052 | 6 restraints |
wR(F2) = 0.145 | H-atom parameters constrained |
S = 1.11 | Δρmax = 0.88 e Å−3 |
4386 reflections | Δρmin = −0.62 e Å−3 |
238 parameters |
x | y | z | Uiso*/Ueq | Occ. (<1) | |
Cd1 | 0.5000 | 0.83464 (7) | 0.2500 | 0.03522 (16) | 0.856 (2) |
Cd1' | 0.5000 | 0.6668 (5) | 0.2500 | 0.0545 (12) | 0.144 (2) |
O1 | 0.44455 (12) | 0.8964 (4) | 0.37992 (17) | 0.0488 (6) | |
O2 | 0.45034 (12) | 0.5760 (4) | 0.37344 (17) | 0.0508 (6) | |
O1w | 0.40361 (12) | 0.7807 (6) | 0.15998 (19) | 0.0725 (10) | |
H1w1 | 0.3597 | 0.7741 | 0.1660 | 0.087* | |
H1w2 | 0.4116 | 0.7753 | 0.1013 | 0.087* | |
O2w | 0.5000 | 1.2162 (7) | 0.2500 | 0.0726 (12) | |
H2w1 | 0.4831 | 1.2922 | 0.2920 | 0.087* | |
O3w | 0.41291 (12) | 0.7615 (4) | −0.02930 (18) | 0.0499 (6) | |
H3w1 | 0.4292 | 0.8643 | −0.0557 | 0.060* | |
H3w2 | 0.4306 | 0.6557 | −0.0509 | 0.060* | |
N1 | 0.25822 (12) | 0.7573 (4) | 0.15794 (19) | 0.0381 (6) | |
N2 | 0.15315 (13) | 0.7540 (5) | 0.06446 (19) | 0.0413 (6) | |
N3 | 0.25850 (14) | 0.7558 (6) | −0.0040 (2) | 0.0568 (9) | |
H3N1 | 0.2369 | 0.7547 | −0.0577 | 0.068* | |
H3N2 | 0.3031 | 0.7570 | −0.0013 | 0.068* | |
N4 | 0.18959 (12) | 0.7447 (4) | −0.19967 (18) | 0.0374 (6) | |
N5 | 0.09175 (13) | 0.7455 (5) | −0.3069 (2) | 0.0426 (6) | |
N6 | 0.07806 (14) | 0.7472 (6) | −0.1467 (2) | 0.0537 (8) | |
H6N1 | 0.0339 | 0.7478 | −0.1565 | 0.064* | |
H6N2 | 0.0949 | 0.7475 | −0.0901 | 0.064* | |
C1 | 0.43394 (16) | 0.7257 (6) | 0.4143 (2) | 0.0433 (8) | |
C2 | 0.4002 (2) | 0.7178 (7) | 0.5091 (3) | 0.0613 (10) | |
H2A | 0.3568 | 0.6487 | 0.5032 | 0.092* | |
H2B | 0.3921 | 0.8498 | 0.5310 | 0.092* | |
H2C | 0.4302 | 0.6500 | 0.5532 | 0.092* | |
C3 | 0.22286 (15) | 0.7559 (5) | 0.0748 (2) | 0.0376 (7) | |
C4 | 0.22067 (15) | 0.7571 (5) | 0.2354 (2) | 0.0383 (7) | |
C5 | 0.14889 (16) | 0.7550 (6) | 0.2313 (2) | 0.0452 (8) | |
H5 | 0.1230 | 0.7541 | 0.2856 | 0.054* | |
C6 | 0.11762 (15) | 0.7543 (6) | 0.1434 (3) | 0.0440 (8) | |
C7 | 0.25937 (18) | 0.7567 (6) | 0.3288 (2) | 0.0479 (8) | |
H7A | 0.2491 | 0.6374 | 0.3621 | 0.072* | |
H7B | 0.2453 | 0.8686 | 0.3651 | 0.072* | |
H7C | 0.3083 | 0.7639 | 0.3185 | 0.072* | |
C8 | 0.03971 (17) | 0.7526 (9) | 0.1313 (3) | 0.0714 (13) | |
H8A | 0.0273 | 0.7562 | 0.0655 | 0.107* | |
H8B | 0.0207 | 0.8660 | 0.1619 | 0.107* | |
H8C | 0.0215 | 0.6345 | 0.1588 | 0.107* | |
C9 | 0.12098 (15) | 0.7459 (5) | −0.2201 (2) | 0.0359 (6) | |
C10 | 0.13499 (17) | 0.7441 (6) | −0.3780 (2) | 0.0452 (8) | |
C11 | 0.20641 (17) | 0.7422 (6) | −0.3641 (2) | 0.0453 (8) | |
H11 | 0.2361 | 0.7409 | −0.4145 | 0.054* | |
C12 | 0.23172 (15) | 0.7423 (5) | −0.2725 (2) | 0.0389 (7) | |
C13 | 0.1036 (2) | 0.7431 (9) | −0.4754 (3) | 0.0721 (13) | |
H13A | 0.0591 | 0.6794 | −0.4748 | 0.108* | |
H13B | 0.1335 | 0.6728 | −0.5167 | 0.108* | |
H13C | 0.0980 | 0.8766 | −0.4972 | 0.108* | |
C14 | 0.30850 (16) | 0.7406 (6) | −0.2523 (3) | 0.0500 (9) | |
H14A | 0.3287 | 0.8597 | −0.2759 | 0.075* | |
H14B | 0.3289 | 0.6286 | −0.2824 | 0.075* | |
H14C | 0.3170 | 0.7325 | −0.1856 | 0.075* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Cd1 | 0.02966 (19) | 0.0508 (3) | 0.0253 (2) | 0.000 | 0.00195 (13) | 0.000 |
Cd1' | 0.0625 (18) | 0.069 (3) | 0.0324 (15) | 0.000 | 0.0009 (11) | 0.000 |
O1 | 0.0517 (12) | 0.0571 (15) | 0.0379 (13) | 0.0050 (11) | 0.0090 (10) | 0.0006 (11) |
O2 | 0.0545 (13) | 0.0566 (16) | 0.0419 (13) | −0.0019 (12) | 0.0081 (11) | −0.0023 (12) |
O1w | 0.0333 (12) | 0.148 (3) | 0.0359 (15) | −0.0059 (14) | 0.0006 (11) | −0.0090 (16) |
O2w | 0.087 (3) | 0.078 (3) | 0.055 (3) | 0.000 | 0.027 (2) | 0.000 |
O3w | 0.0531 (13) | 0.0574 (15) | 0.0396 (14) | −0.0016 (11) | 0.0077 (11) | 0.0011 (11) |
N1 | 0.0328 (12) | 0.0482 (16) | 0.0333 (14) | −0.0005 (10) | −0.0039 (11) | −0.0001 (11) |
N2 | 0.0345 (12) | 0.0579 (17) | 0.0314 (14) | 0.0002 (11) | −0.0023 (11) | −0.0005 (12) |
N3 | 0.0355 (14) | 0.104 (3) | 0.0309 (15) | 0.0007 (15) | 0.0006 (12) | 0.0001 (16) |
N4 | 0.0347 (12) | 0.0457 (15) | 0.0318 (14) | 0.0000 (10) | −0.0014 (11) | 0.0003 (11) |
N5 | 0.0349 (12) | 0.0547 (18) | 0.0380 (15) | −0.0006 (11) | −0.0030 (11) | 0.0006 (12) |
N6 | 0.0380 (14) | 0.086 (2) | 0.0374 (17) | −0.0002 (14) | 0.0036 (13) | 0.0009 (15) |
C1 | 0.0323 (14) | 0.067 (2) | 0.0305 (16) | −0.0023 (14) | 0.0029 (12) | 0.0035 (15) |
C2 | 0.061 (2) | 0.086 (3) | 0.037 (2) | −0.002 (2) | 0.0163 (18) | 0.0017 (19) |
C3 | 0.0350 (14) | 0.0467 (18) | 0.0310 (16) | −0.0012 (12) | −0.0025 (12) | −0.0001 (13) |
C4 | 0.0378 (15) | 0.0460 (18) | 0.0309 (16) | 0.0001 (12) | −0.0018 (13) | 0.0004 (13) |
C5 | 0.0357 (15) | 0.066 (2) | 0.0342 (17) | −0.0004 (14) | 0.0036 (14) | −0.0015 (15) |
C6 | 0.0311 (14) | 0.059 (2) | 0.0412 (19) | 0.0010 (13) | −0.0031 (13) | 0.0003 (15) |
C7 | 0.0461 (17) | 0.065 (2) | 0.0317 (17) | 0.0006 (15) | −0.0072 (14) | −0.0021 (15) |
C8 | 0.0298 (16) | 0.135 (4) | 0.050 (2) | −0.002 (2) | 0.0001 (16) | 0.001 (2) |
C9 | 0.0352 (14) | 0.0381 (16) | 0.0344 (16) | −0.0014 (11) | −0.0004 (12) | −0.0009 (12) |
C10 | 0.0423 (16) | 0.057 (2) | 0.0358 (18) | −0.0003 (14) | −0.0073 (14) | −0.0005 (15) |
C11 | 0.0412 (16) | 0.061 (2) | 0.0333 (17) | 0.0005 (14) | 0.0031 (14) | −0.0018 (15) |
C12 | 0.0340 (14) | 0.0457 (18) | 0.0367 (17) | −0.0013 (12) | −0.0008 (13) | −0.0005 (13) |
C13 | 0.059 (2) | 0.121 (4) | 0.035 (2) | 0.002 (2) | −0.0132 (18) | 0.001 (2) |
C14 | 0.0323 (14) | 0.071 (3) | 0.046 (2) | 0.0003 (14) | 0.0012 (14) | 0.0011 (17) |
Cd1—O1 | 2.198 (2) | N5—C9 | 1.345 (4) |
Cd1—O1i | 2.198 (2) | N6—C9 | 1.348 (4) |
Cd1—O2 | 2.674 (2) | N6—H6N1 | 0.8600 |
Cd1—O2i | 2.674 (2) | N6—H6N2 | 0.8600 |
Cd1—O1w | 2.260 (3) | C1—C2 | 1.513 (5) |
Cd1—O1wi | 2.260 (3) | C2—H2A | 0.9600 |
Cd1—O2w | 2.583 (5) | C2—H2B | 0.9600 |
Cd1'—O2i | 2.113 (3) | C2—H2C | 0.9600 |
Cd1'—O2 | 2.113 (3) | C4—C5 | 1.384 (4) |
Cd1'—O1wi | 2.360 (3) | C4—C7 | 1.507 (4) |
Cd1'—O1w | 2.360 (3) | C5—C6 | 1.375 (5) |
Cd1'—C1 | 2.719 (3) | C5—H5 | 0.9300 |
Cd1'—C1i | 2.719 (3) | C6—C8 | 1.508 (4) |
C1—O1 | 1.274 (5) | C7—H7A | 0.9600 |
C1—O2 | 1.214 (5) | C7—H7B | 0.9600 |
O1w—H1w1 | 0.85 | C7—H7C | 0.9600 |
O1w—H1w2 | 0.85 | C8—H8A | 0.9600 |
O2w—H2w1 | 0.86 | C8—H8B | 0.9600 |
O3w—H3w1 | 0.85 | C8—H8C | 0.9600 |
O3w—H3w2 | 0.85 | C10—C11 | 1.387 (5) |
N1—C4 | 1.334 (4) | C10—C13 | 1.499 (5) |
N1—C3 | 1.350 (4) | C11—C12 | 1.379 (5) |
N2—C6 | 1.330 (4) | C11—H11 | 0.9300 |
N2—C3 | 1.349 (4) | C12—C14 | 1.502 (4) |
N3—C3 | 1.330 (4) | C13—H13A | 0.9600 |
N3—H3N1 | 0.8600 | C13—H13B | 0.9600 |
N3—H3N2 | 0.8600 | C13—H13C | 0.9600 |
N4—C12 | 1.332 (4) | C14—H14A | 0.9600 |
N4—C9 | 1.348 (4) | C14—H14B | 0.9600 |
N5—C10 | 1.326 (4) | C14—H14C | 0.9600 |
Cd1'—Cd1—O1 | 100.96 (7) | H2B—C2—H2C | 109.5 |
Cd1'—Cd1—O1i | 100.96 (7) | N3—C3—N2 | 116.3 (3) |
O1—Cd1—O1i | 158.07 (15) | N3—C3—N1 | 118.6 (3) |
Cd1'—Cd1—O1wi | 80.71 (11) | N2—C3—N1 | 125.2 (3) |
O1—Cd1—O1wi | 88.00 (9) | N1—C4—C5 | 121.9 (3) |
O1i—Cd1—O1wi | 95.53 (9) | N1—C4—C7 | 117.4 (3) |
O1—Cd1—O1w | 95.53 (9) | C5—C4—C7 | 120.6 (3) |
O1i—Cd1—O1w | 88.00 (9) | C6—C5—C4 | 117.0 (3) |
O1wi—Cd1—O1w | 161.4 (2) | C6—C5—H5 | 121.5 |
O1—Cd1—O2w | 79.04 (7) | C4—C5—H5 | 121.5 |
O1i—Cd1—O2w | 79.04 (7) | N2—C6—C5 | 123.0 (3) |
O1wi—Cd1—O2w | 99.29 (11) | N2—C6—C8 | 115.9 (3) |
O1w—Cd1—O2w | 99.29 (11) | C5—C6—C8 | 121.1 (3) |
O2i—Cd1'—O2 | 146.2 (2) | C4—C7—H7A | 109.5 |
O2i—Cd1'—O1wi | 100.29 (9) | C4—C7—H7B | 109.5 |
O2—Cd1'—O1wi | 90.67 (9) | H7A—C7—H7B | 109.5 |
O2i—Cd1'—O1w | 90.67 (9) | C4—C7—H7C | 109.5 |
O2—Cd1'—O1w | 100.29 (9) | H7A—C7—H7C | 109.5 |
O1wi—Cd1'—O1w | 141.9 (3) | H7B—C7—H7C | 109.5 |
C1—O1—Cd1 | 103.7 (2) | C6—C8—H8A | 109.5 |
C1—O2—Cd1' | 106.5 (3) | C6—C8—H8B | 109.5 |
Cd1—O1w—H1w1 | 139.0 | H8A—C8—H8B | 109.5 |
Cd1'—O1w—H1w1 | 134.2 | C6—C8—H8C | 109.5 |
Cd1—O1w—H1w2 | 113.3 | H8A—C8—H8C | 109.5 |
Cd1'—O1w—H1w2 | 111.0 | H8B—C8—H8C | 109.5 |
H1w1—O1w—H1w2 | 107.5 | N5—C9—N4 | 125.8 (3) |
Cd1—O2w—H2w1 | 126.8 | N5—C9—N6 | 117.4 (3) |
H3w1—O3w—H3w2 | 111.8 | N4—C9—N6 | 116.9 (3) |
C4—N1—C3 | 116.8 (3) | N5—C10—C11 | 122.2 (3) |
C6—N2—C3 | 116.2 (3) | N5—C10—C13 | 117.2 (3) |
C3—N3—H3N1 | 120.0 | C11—C10—C13 | 120.6 (3) |
C3—N3—H3N2 | 120.0 | C12—C11—C10 | 117.5 (3) |
H3N1—N3—H3N2 | 120.0 | C12—C11—H11 | 121.3 |
C12—N4—C9 | 116.6 (3) | C10—C11—H11 | 121.3 |
C10—N5—C9 | 116.3 (3) | N4—C12—C11 | 121.7 (3) |
C9—N6—H6N1 | 120.0 | N4—C12—C14 | 118.0 (3) |
C9—N6—H6N2 | 120.0 | C11—C12—C14 | 120.3 (3) |
H6N1—N6—H6N2 | 120.0 | C10—C13—H13A | 109.5 |
O2—C1—O1 | 121.8 (3) | C10—C13—H13B | 109.5 |
O2—C1—C2 | 121.4 (4) | H13A—C13—H13B | 109.5 |
O1—C1—C2 | 116.8 (3) | C10—C13—H13C | 109.5 |
O2—C1—Cd1' | 48.15 (19) | H13A—C13—H13C | 109.5 |
O1—C1—Cd1' | 73.72 (19) | H13B—C13—H13C | 109.5 |
C2—C1—Cd1' | 169.2 (3) | C12—C14—H14A | 109.5 |
C1—C2—H2A | 109.5 | C12—C14—H14B | 109.5 |
C1—C2—H2B | 109.5 | H14A—C14—H14B | 109.5 |
H2A—C2—H2B | 109.5 | C12—C14—H14C | 109.5 |
C1—C2—H2C | 109.5 | H14A—C14—H14C | 109.5 |
H2A—C2—H2C | 109.5 | H14B—C14—H14C | 109.5 |
O1i—Cd1—O1—C1 | −176.9 (2) | C7—C4—C5—C6 | −179.6 (3) |
O1wi—Cd1—O1—C1 | −77.0 (2) | C3—N2—C6—C5 | −0.5 (6) |
O1w—Cd1—O1—C1 | 84.7 (2) | C3—N2—C6—C8 | 179.9 (4) |
O2w—Cd1—O1—C1 | −176.9 (2) | C4—C5—C6—N2 | 0.5 (6) |
O2i—Cd1'—O2—C1 | 180.0 (2) | C4—C5—C6—C8 | −179.8 (4) |
O1wi—Cd1'—O2—C1 | 70.2 (2) | C10—N5—C9—N4 | −0.1 (5) |
O1w—Cd1'—O2—C1 | −73.1 (3) | C10—N5—C9—N6 | 180.0 (3) |
Cd1'—O2—C1—O1 | 2.9 (4) | C12—N4—C9—N5 | −0.2 (5) |
Cd1'—O2—C1—C2 | −176.8 (3) | C12—N4—C9—N6 | 179.7 (3) |
Cd1—O1—C1—O2 | −3.6 (4) | C9—N5—C10—C11 | 0.3 (5) |
Cd1—O1—C1—C2 | 176.1 (2) | C9—N5—C10—C13 | 179.9 (4) |
C6—N2—C3—N3 | −179.9 (4) | N5—C10—C11—C12 | −0.2 (6) |
C6—N2—C3—N1 | 0.2 (5) | C13—C10—C11—C12 | −179.7 (4) |
C4—N1—C3—N3 | −179.9 (3) | C9—N4—C12—C11 | 0.4 (5) |
C4—N1—C3—N2 | −0.1 (5) | C9—N4—C12—C14 | −179.9 (3) |
C3—N1—C4—C5 | 0.1 (5) | C10—C11—C12—N4 | −0.2 (6) |
C3—N1—C4—C7 | 179.4 (3) | C10—C11—C12—C14 | −179.9 (3) |
N1—C4—C5—C6 | −0.3 (6) |
Symmetry code: (i) −x+1, y, −z+1/2. |
D—H···A | D—H | H···A | D···A | D—H···A |
O1w—H1w1···N1 | 0.85 | 1.96 | 2.808 (3) | 171 |
O1w—H1w2···O3w | 0.85 | 1.86 | 2.706 (4) | 170 |
O2w—H2w1···O2ii | 0.86 | 2.34 | 3.165 (5) | 162 |
O3w—H3w1···O1iii | 0.85 | 1.89 | 2.728 (4) | 167 |
O3w—H3w2···O2iv | 0.85 | 1.95 | 2.776 (4) | 164 |
N3—H3n1···N4 | 0.86 | 2.20 | 3.055 (4) | 176 |
N3—H3n2···O3w | 0.86 | 2.17 | 3.009 (4) | 167 |
N6—H6n1···N5v | 0.86 | 2.47 | 3.324 (4) | 177 |
N6—H6n2···N2 | 0.86 | 2.44 | 3.302 (4) | 175 |
Symmetry codes: (ii) x, y+1, z; (iii) x, −y+2, z−1/2; (iv) x, −y+1, z−1/2; (v) −x, y, −z−1/2. |
Experimental details
Crystal data | |
Chemical formula | [Cd(C2H3O2)2(H2O)3]·4C6H9N3·2H2O |
Mr | 813.22 |
Crystal system, space group | Monoclinic, P2/c |
Temperature (K) | 295 |
a, b, c (Å) | 19.287 (1), 6.7697 (4), 14.2238 (4) |
β (°) | 91.444 (1) |
V (Å3) | 1856.56 (16) |
Z | 2 |
Radiation type | Mo Kα |
µ (mm−1) | 0.65 |
Crystal size (mm) | 0.40 × 0.20 × 0.16 |
Data collection | |
Diffractometer | Bruker APEX CCD |
Absorption correction | Multi-scan (SADABS; Sheldrick, 1996) |
Tmin, Tmax | 0.567, 0.903 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 13020, 4386, 3794 |
Rint | 0.053 |
(sin θ/λ)max (Å−1) | 0.665 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.052, 0.145, 1.11 |
No. of reflections | 4386 |
No. of parameters | 238 |
No. of restraints | 6 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 0.88, −0.62 |
Computer programs: SMART (Bruker, 2004), SAINT (Bruker, 2004), SAINT, SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), X-SEED (Barbour, 2001), publCIF (Westrip, 2007).
Cd1—O1 | 2.198 (2) | Cd1—O2w | 2.583 (5) |
Cd1—O2 | 2.674 (2) | C1—O1 | 1.274 (5) |
Cd1—O1w | 2.260 (3) | C1—O2 | 1.214 (5) |
D—H···A | D—H | H···A | D···A | D—H···A |
O1w—H1w1···N1 | 0.85 | 1.96 | 2.808 (3) | 171 |
O1w—H1w2···O3w | 0.85 | 1.86 | 2.706 (4) | 170 |
O2w—H2w1···O2i | 0.86 | 2.34 | 3.165 (5) | 162 |
O3w—H3w1···O1ii | 0.85 | 1.89 | 2.728 (4) | 167 |
O3w—H3w2···O2iii | 0.85 | 1.95 | 2.776 (4) | 164 |
N3—H3n1···N4 | 0.86 | 2.20 | 3.055 (4) | 176 |
N3—H3n2···O3w | 0.86 | 2.17 | 3.009 (4) | 167 |
N6—H6n1···N5iv | 0.86 | 2.47 | 3.324 (4) | 177 |
N6—H6n2···N2 | 0.86 | 2.44 | 3.302 (4) | 175 |
Symmetry codes: (i) x, y+1, z; (ii) x, −y+2, z−1/2; (iii) x, −y+1, z−1/2; (iv) −x, y, −z−1/2. |
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Cadmium acetate forms adducts with nitrogen-donor ligands and among the known crystal structures of such materials are the bis(4-aminophenyl)methane (Wang et al., 2004), 2,2'-bipyridine (Ye et al., 2000) and diethylnicotinamide (Sergienko et al., 1980) adducts.
The title compound, (I), the product of the reaction of cadmium acetate with 2-amino-4,6-pyrimidine, has the N-heterocycle engaging instead in an outer-sphere type of coordination (i.e. interacting indirectly through hydrogen bonds). Compound (I) consists of a triaquadiacetatocadmium molecule (Cd site symmetry 2) along with an uncoordinated water molecule and two N-heterocycles (Fig. 1). The cadmium atom is five-coordinate, but the geometry is distorted towards a pentagonal bipyramid owing to two long Cd···O interactions (Table 1). Hydrogen bonds link the three entities into a three-dimensional network motif (Table 2).