Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S160053680703927X/lh2474sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S160053680703927X/lh2474Isup2.hkl |
CCDC reference: 660092
Key indicators
- Single-crystal X-ray study
- T = 295 K
- Mean (C-C) = 0.007 Å
- Disorder in main residue
- R factor = 0.048
- wR factor = 0.151
- Data-to-parameter ratio = 13.4
checkCIF/PLATON results
No syntax errors found
Alert level B PLAT414_ALERT_2_B Short Intra D-H..H-X H5 .. H1N2 .. 1.88 Ang. PLAT731_ALERT_1_B Bond Calc 0.85(5), Rep 0.850(10) ...... 5.00 su-Ra O1W -H1W2 1.555 1.555 PLAT731_ALERT_1_B Bond Calc 0.86(5), Rep 0.850(10) ...... 5.00 su-Ra O2W -H2W2 1.555 1.555 PLAT735_ALERT_1_B D-H Calc 0.85(5), Rep 0.850(10) ...... 5.00 su-Ra O1W -H2# 1.555 1.555 PLAT735_ALERT_1_B D-H Calc 0.86(5), Rep 0.850(10) ...... 5.00 su-Ra O2W -H4# 1.555 1.555 PLAT736_ALERT_1_B H...A Calc 1.98(5), Rep 1.980(10) ...... 5.00 su-Ra H2# -O3 1.555 2.655 PLAT736_ALERT_1_B H...A Calc 1.93(5), Rep 1.930(10) ...... 5.00 su-Ra H4# -O3 1.555 4.576
Alert level C PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT094_ALERT_2_C Ratio of Maximum / Minimum Residual Density .... 2.37 PLAT152_ALERT_1_C Supplied and Calc Volume s.u. Inconsistent ..... ? PLAT301_ALERT_3_C Main Residue Disorder ......................... 13.00 Perc. PLAT711_ALERT_1_C BOND Unknown or Inconsistent Label .......... O1<I>W< CD1 O1<I>W< PLAT711_ALERT_1_C BOND Unknown or Inconsistent Label .......... O2<I>W< CD1 O2<I>W< PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 8 PLAT731_ALERT_1_C Bond Calc 0.85(4), Rep 0.850(10) ...... 4.00 su-Ra O1W -H1W1 1.555 1.555 PLAT731_ALERT_1_C Bond Calc 0.85(4), Rep 0.850(10) ...... 4.00 su-Ra O2W -H2W1 1.555 1.555 PLAT735_ALERT_1_C D-H Calc 0.85(4), Rep 0.850(10) ...... 4.00 su-Ra O1W -H1# 1.555 1.555 PLAT735_ALERT_1_C D-H Calc 0.85(4), Rep 0.850(10) ...... 4.00 su-Ra O2W -H3# 1.555 1.555 PLAT736_ALERT_1_C H...A Calc 2.02(4), Rep 2.020(10) ...... 4.00 su-Ra H3# -O3 1.555 3.666
Alert level G PLAT860_ALERT_3_G Note: Number of Least-Squares Restraints ....... 6
0 ALERT level A = In general: serious problem 7 ALERT level B = Potentially serious problem 12 ALERT level C = Check and explain 1 ALERT level G = General alerts; check 15 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 2 ALERT type 2 Indicator that the structure model may be wrong or deficient 2 ALERT type 3 Indicator that the structure quality may be low 1 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check
For literature on metal 4-formylbenzoates, see, for example: Deng et al. (2006a,b).
Cadmium diacetate dihydrate (0.133 g, 0.5 mmol) was added to an aqueous solution of 4-formylbenzoic acid (0.15 g, 1 mmol) and nicotinamide (0.122 g, 1 mmol). The pH value of the mixture was about 5. The solution was set aside for the growth of colorless prismatic crystals. CH&N elemental analysis. Calc. for C28H30N4O12Cd: C 46.26, H 4.16, N 7.71%. Found: C 46.24, H 4.11, N 7.76%.
The amido and formyl parts are disordered over two positions; the occupancies refined to a 0.59 (1):0.41 ratio for both groups. The C6—O1 and C6—O1' bond distances were restrained to within 0.01 Å of each other, as were the C6—N1 and C6—N1' distances. The carbon- and nitrogen bound H atoms were generated geometrically (C—H 0.93, N—H 0.86 Å) and were included in the refinement in the riding-model approximation, with U(H) set to 1.2Ueq(C,N). The water H atoms were located in a difference Fourier map, and were refined with a distance restraint of O—H 0.85 (1) Å; their Uiso(H) values were freely refined. The final difference Fourier map had a large peak at about 1 Å from O3, but was otherwise diffuse.
Cadmium bis(4-formylbenzoate) forms a hydrated 1:2 adduct with imidazole; in the crystal structure, two molecules are linked by two Cd—Ocarboxyl interactions into a dinuclear species. The formylbenzoate anion functions in a chelating mode (Deng et al., 2006a). With the larger benzimidazole ligand, a 1:1 aqua adduct is formed, and one carboxylate anion is bidentate whereas the other is monodentate in the seven-coordinate structure (Deng et al., 2006b). Replacing the N-heterocycle by nicotinamide furnishes the title compound as a salt whose cation has two nicotinamide ligands binding to the tetraaquacadmium group; the carboxylate group is displaced from the coordination sphere and it exists as a free anion (Fig. 1). Hydrogen bonds link the cation and anion into a three-dimensional network.
For literature on metal 4-formylbenzoates, see, for example: Deng et al. (2006a,b).
Data collection: RAPID-AUTO (Rigaku, 1998); cell refinement: RAPID-AUTO; data reduction: CrystalStructure (Rigaku/MSC, 2002); 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(C6H6N2O)2(H2O)4](C8H5O3)2 | F(000) = 740 |
Mr = 726.96 | Dx = 1.657 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ybc | Cell parameters from 10447 reflections |
a = 14.922 (1) Å | θ = 3.1–27.5° |
b = 7.0382 (4) Å | µ = 0.82 mm−1 |
c = 14.030 (1) Å | T = 295 K |
β = 98.634 (2)° | Prism, colourless |
V = 1456.8 (2) Å3 | 0.35 × 0.24 × 0.18 mm |
Z = 2 |
Rigaku R-AXIS RAPID IP diffractometer | 3332 independent reflections |
Radiation source: fine-focus sealed tube | 2816 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.035 |
ω scans | θmax = 27.5°, θmin = 3.1° |
Absorption correction: multi-scan (ABSCOR; Higashi, 1995) | h = −19→19 |
Tmin = 0.680, Tmax = 0.866 | k = −9→8 |
13559 measured reflections | l = −17→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)] = 0.048 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.151 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.14 | w = 1/[σ2(Fo2) + (0.0584P)2 + 5.994P] where P = (Fo2 + 2Fc2)/3 |
3332 reflections | (Δ/σ)max = 0.001 |
249 parameters | Δρmax = 1.08 e Å−3 |
6 restraints | Δρmin = −0.46 e Å−3 |
[Cd(C6H6N2O)2(H2O)4](C8H5O3)2 | V = 1456.8 (2) Å3 |
Mr = 726.96 | Z = 2 |
Monoclinic, P21/c | Mo Kα radiation |
a = 14.922 (1) Å | µ = 0.82 mm−1 |
b = 7.0382 (4) Å | T = 295 K |
c = 14.030 (1) Å | 0.35 × 0.24 × 0.18 mm |
β = 98.634 (2)° |
Rigaku R-AXIS RAPID IP diffractometer | 3332 independent reflections |
Absorption correction: multi-scan (ABSCOR; Higashi, 1995) | 2816 reflections with I > 2σ(I) |
Tmin = 0.680, Tmax = 0.866 | Rint = 0.035 |
13559 measured reflections |
R[F2 > 2σ(F2)] = 0.048 | 6 restraints |
wR(F2) = 0.151 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.14 | Δρmax = 1.08 e Å−3 |
3332 reflections | Δρmin = −0.46 e Å−3 |
249 parameters |
x | y | z | Uiso*/Ueq | Occ. (<1) | |
Cd1 | 0.5000 | 0.5000 | 0.5000 | 0.03018 (17) | |
O1W | 0.4608 (3) | 0.7588 (6) | 0.4012 (3) | 0.0380 (8) | |
H1W1 | 0.415 (2) | 0.739 (9) | 0.359 (3) | 0.042 (16)* | |
H1W2 | 0.498 (3) | 0.835 (7) | 0.381 (4) | 0.046 (18)* | |
O2W | 0.5403 (3) | 0.6836 (6) | 0.6390 (3) | 0.0429 (9) | |
H2W1 | 0.550 (4) | 0.626 (8) | 0.693 (2) | 0.047 (17)* | |
H2W2 | 0.503 (3) | 0.771 (7) | 0.649 (5) | 0.053 (19)* | |
O1 | 0.9598 (11) | 0.607 (3) | 0.579 (2) | 0.059 (5) | 0.589 (12) |
N1 | 0.8621 (11) | 0.553 (2) | 0.6850 (11) | 0.047 (3) | 0.589 (12) |
H1N1 | 0.9056 | 0.5424 | 0.7325 | 0.056* | 0.589 (12) |
H1N2 | 0.8068 | 0.5408 | 0.6945 | 0.056* | 0.589 (12) |
O1' | 0.8628 (13) | 0.638 (2) | 0.6856 (12) | 0.045 (4) | 0.411 (12) |
N1' | 0.9589 (15) | 0.547 (5) | 0.587 (3) | 0.048 (7) | 0.411 (12) |
H1N3 | 1.0032 | 0.5548 | 0.6338 | 0.057* | 0.411 (12) |
H1N4 | 0.9687 | 0.5133 | 0.5307 | 0.057* | 0.411 (12) |
O2 | 0.3258 (3) | 0.6507 (8) | 0.2597 (3) | 0.0641 (14) | |
O3 | 0.4294 (3) | 0.5203 (6) | 0.1818 (3) | 0.0447 (9) | |
O4 | 0.0030 (5) | 0.6015 (14) | −0.1545 (5) | 0.061 (3) | 0.589 (12) |
O4' | 0.1012 (6) | 0.5493 (16) | −0.2424 (6) | 0.044 (3) | 0.411 (12) |
N2 | 0.6443 (3) | 0.5390 (6) | 0.4632 (3) | 0.0329 (9) | |
C1 | 0.6592 (3) | 0.5775 (7) | 0.3732 (4) | 0.0348 (10) | |
H1 | 0.6104 | 0.5721 | 0.3235 | 0.042* | |
C2 | 0.7431 (4) | 0.6246 (8) | 0.3510 (3) | 0.0376 (11) | |
H2 | 0.7504 | 0.6553 | 0.2881 | 0.045* | |
C3 | 0.8166 (3) | 0.6255 (8) | 0.4242 (4) | 0.0352 (10) | |
H3 | 0.8743 | 0.6539 | 0.4108 | 0.042* | |
C4 | 0.8033 (3) | 0.5835 (7) | 0.5178 (3) | 0.0303 (9) | |
C5 | 0.7159 (3) | 0.5422 (7) | 0.5338 (3) | 0.0320 (10) | |
H5 | 0.7065 | 0.5154 | 0.5964 | 0.038* | |
C6 | 0.8796 (3) | 0.5866 (8) | 0.6012 (4) | 0.0388 (11) | |
C7 | 0.3503 (4) | 0.5841 (8) | 0.1864 (3) | 0.0361 (11) | |
C8 | 0.2813 (3) | 0.5820 (7) | 0.0956 (3) | 0.0314 (9) | |
C9 | 0.3067 (4) | 0.5421 (7) | 0.0065 (4) | 0.0361 (11) | |
H9 | 0.3667 | 0.5124 | 0.0025 | 0.043* | |
C10 | 0.2440 (4) | 0.5460 (8) | −0.0759 (4) | 0.0400 (12) | |
H10 | 0.2625 | 0.5257 | −0.1355 | 0.048* | |
C11 | 0.1527 (3) | 0.5804 (8) | −0.0705 (4) | 0.0360 (10) | |
C12 | 0.1262 (4) | 0.6195 (8) | 0.0193 (4) | 0.0414 (12) | |
H12 | 0.0656 | 0.6429 | 0.0240 | 0.050* | |
C13 | 0.1909 (3) | 0.6228 (8) | 0.1008 (4) | 0.0375 (11) | |
H13 | 0.1737 | 0.6527 | 0.1601 | 0.045* | |
C14 | 0.0842 (4) | 0.5798 (9) | −0.1583 (4) | 0.0465 (13) | |
H14 | 0.1030 | 0.5625 | −0.2179 | 0.056* | 0.589 (12) |
H14' | 0.0243 | 0.6036 | −0.1510 | 0.056* | 0.411 (12) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Cd1 | 0.0234 (2) | 0.0379 (3) | 0.0283 (2) | −0.0023 (2) | 0.00111 (16) | 0.0026 (2) |
O1W | 0.039 (2) | 0.040 (2) | 0.0349 (18) | 0.0032 (17) | 0.0037 (15) | 0.0051 (16) |
O2W | 0.046 (2) | 0.041 (2) | 0.039 (2) | 0.0073 (18) | −0.0027 (17) | −0.0019 (17) |
O1 | 0.029 (5) | 0.090 (15) | 0.061 (7) | −0.017 (6) | 0.009 (5) | −0.013 (10) |
N1 | 0.030 (4) | 0.066 (9) | 0.039 (5) | −0.013 (7) | −0.009 (4) | 0.006 (6) |
O1' | 0.041 (6) | 0.058 (10) | 0.034 (6) | −0.011 (8) | 0.003 (4) | 0.006 (7) |
N1' | 0.026 (8) | 0.058 (16) | 0.053 (12) | 0.000 (8) | −0.013 (7) | −0.008 (11) |
O2 | 0.058 (3) | 0.100 (4) | 0.0311 (19) | 0.025 (3) | −0.0045 (18) | −0.005 (2) |
O3 | 0.045 (2) | 0.044 (2) | 0.044 (2) | 0.0017 (17) | −0.0005 (16) | −0.0002 (17) |
O4 | 0.034 (4) | 0.107 (7) | 0.039 (4) | −0.010 (4) | −0.010 (3) | −0.007 (4) |
O4' | 0.028 (4) | 0.075 (7) | 0.027 (4) | 0.010 (4) | 0.000 (3) | 0.000 (4) |
N2 | 0.0265 (19) | 0.037 (2) | 0.035 (2) | −0.0021 (16) | 0.0027 (16) | 0.0034 (17) |
C1 | 0.035 (2) | 0.035 (2) | 0.033 (2) | 0.003 (2) | 0.0001 (19) | −0.002 (2) |
C2 | 0.043 (3) | 0.043 (3) | 0.029 (2) | 0.007 (2) | 0.011 (2) | −0.001 (2) |
C3 | 0.030 (2) | 0.039 (3) | 0.039 (3) | 0.000 (2) | 0.0111 (19) | 0.001 (2) |
C4 | 0.025 (2) | 0.032 (2) | 0.033 (2) | 0.0003 (19) | 0.0017 (17) | −0.0002 (19) |
C5 | 0.029 (2) | 0.037 (3) | 0.030 (2) | 0.0011 (19) | 0.0039 (18) | 0.0063 (19) |
C6 | 0.028 (2) | 0.043 (3) | 0.043 (3) | −0.003 (2) | 0.001 (2) | 0.000 (2) |
C7 | 0.040 (3) | 0.040 (3) | 0.028 (2) | −0.002 (2) | 0.005 (2) | 0.005 (2) |
C8 | 0.036 (2) | 0.027 (2) | 0.031 (2) | −0.004 (2) | 0.0028 (19) | 0.0007 (19) |
C9 | 0.035 (2) | 0.040 (3) | 0.034 (2) | −0.002 (2) | 0.009 (2) | 0.003 (2) |
C10 | 0.044 (3) | 0.043 (3) | 0.033 (2) | 0.000 (2) | 0.009 (2) | −0.002 (2) |
C11 | 0.035 (2) | 0.032 (2) | 0.040 (3) | −0.005 (2) | 0.003 (2) | 0.001 (2) |
C12 | 0.033 (2) | 0.046 (3) | 0.045 (3) | 0.001 (2) | 0.003 (2) | −0.007 (2) |
C13 | 0.040 (3) | 0.038 (3) | 0.035 (2) | 0.001 (2) | 0.010 (2) | −0.002 (2) |
C14 | 0.043 (3) | 0.050 (3) | 0.045 (3) | −0.005 (3) | −0.001 (2) | −0.003 (3) |
Cd1—N2 | 2.305 (4) | C1—C2 | 1.376 (7) |
Cd1—N2i | 2.305 (4) | C1—H1 | 0.9300 |
Cd1—O1wi | 2.311 (4) | C2—C3 | 1.385 (7) |
Cd1—O1w | 2.311 (4) | C2—H2 | 0.9300 |
Cd1—O2w | 2.342 (4) | C3—C4 | 1.389 (7) |
Cd1—O2wi | 2.342 (4) | C3—H3 | 0.9300 |
O1W—H1W1 | 0.85 (1) | C4—C5 | 1.387 (6) |
O1W—H1W2 | 0.85 (1) | C4—C6 | 1.505 (7) |
O2W—H2W1 | 0.85 (1) | C5—H5 | 0.9300 |
O2W—H2W2 | 0.85 (1) | C7—C8 | 1.512 (7) |
O1—C6 | 1.289 (15) | C8—C9 | 1.388 (7) |
N1—C6 | 1.264 (16) | C8—C13 | 1.392 (7) |
N1—H1N1 | 0.8600 | C9—C10 | 1.373 (8) |
N1—H1N2 | 0.8600 | C9—H9 | 0.9300 |
O1'—C6 | 1.299 (15) | C10—C11 | 1.397 (7) |
N1'—C6 | 1.259 (19) | C10—H10 | 0.9300 |
N1'—H1N3 | 0.8600 | C11—C12 | 1.404 (7) |
N1'—H1N4 | 0.8600 | C11—C14 | 1.477 (7) |
O2—C7 | 1.235 (6) | C12—C13 | 1.381 (7) |
O3—C7 | 1.274 (7) | C12—H12 | 0.9300 |
O4—C14 | 1.231 (9) | C13—H13 | 0.9300 |
O4'—C14 | 1.263 (10) | C14—H14 | 0.9300 |
N2—C1 | 1.342 (6) | C14—H14' | 0.9300 |
N2—C5 | 1.344 (6) | ||
N2—Cd1—N2i | 180.00 (5) | C5—C4—C6 | 119.8 (4) |
N2—Cd1—O1Wi | 93.85 (14) | C3—C4—C6 | 122.2 (4) |
N2i—Cd1—O1Wi | 86.15 (14) | N2—C5—C4 | 123.2 (4) |
N2—Cd1—O1W | 86.15 (14) | N2—C5—H5 | 118.4 |
N2i—Cd1—O1W | 93.85 (14) | C4—C5—H5 | 118.4 |
O1Wi—Cd1—O1W | 180.00 (15) | N1'—C6—N1 | 116 (2) |
N2—Cd1—O2W | 89.39 (15) | N1—C6—O1 | 125.1 (15) |
N2i—Cd1—O2W | 90.61 (15) | N1'—C6—O1' | 121 (2) |
O1Wi—Cd1—O2W | 85.69 (14) | O1—C6—O1' | 120.1 (15) |
O1W—Cd1—O2W | 94.31 (14) | N1'—C6—C4 | 120 (2) |
N2—Cd1—O2Wi | 90.61 (15) | N1—C6—C4 | 118.9 (8) |
N2i—Cd1—O2Wi | 89.39 (15) | O1—C6—C4 | 115.7 (13) |
O1Wi—Cd1—O2Wi | 94.31 (14) | O1'—C6—C4 | 119.0 (9) |
O1W—Cd1—O2Wi | 85.69 (14) | O2—C7—O3 | 124.6 (5) |
O2W—Cd1—O2Wi | 180.0 | O2—C7—C8 | 117.1 (5) |
Cd1—O1W—H1W1 | 113 (4) | O3—C7—C8 | 118.3 (4) |
Cd1—O1W—H1W2 | 126 (4) | C9—C8—C13 | 119.0 (5) |
H1W1—O1W—H1W2 | 111 (6) | C9—C8—C7 | 121.1 (4) |
Cd1—O2W—H2W1 | 118 (5) | C13—C8—C7 | 119.8 (4) |
Cd1—O2W—H2W2 | 116 (5) | C10—C9—C8 | 120.7 (5) |
H2W1—O2W—H2W2 | 103 (6) | C10—C9—H9 | 119.6 |
C6—N1—H1N1 | 120.0 | C8—C9—H9 | 119.6 |
C6—N1—H1N2 | 120.0 | C9—C10—C11 | 120.3 (5) |
H1N1—N1—H1N2 | 120.0 | C9—C10—H10 | 119.8 |
C6—N1'—H1N3 | 120.0 | C11—C10—H10 | 119.8 |
C6—N1'—H1N4 | 120.0 | C10—C11—C12 | 119.4 (5) |
H1N3—N1'—H1N4 | 120.0 | C10—C11—C14 | 120.9 (5) |
C1—N2—C5 | 117.7 (4) | C12—C11—C14 | 119.7 (5) |
C1—N2—Cd1 | 121.8 (3) | C13—C12—C11 | 119.3 (5) |
C5—N2—Cd1 | 120.2 (3) | C13—C12—H12 | 120.3 |
N2—C1—C2 | 123.1 (5) | C11—C12—H12 | 120.3 |
N2—C1—H1 | 118.4 | C12—C13—C8 | 121.1 (5) |
C2—C1—H1 | 118.4 | C12—C13—H13 | 119.5 |
C1—C2—C3 | 118.7 (5) | C8—C13—H13 | 119.5 |
C1—C2—H2 | 120.7 | O4—C14—C11 | 121.8 (6) |
C3—C2—H2 | 120.7 | O4'—C14—C11 | 124.6 (6) |
C2—C3—C4 | 119.3 (4) | O4—C14—H14 | 119.1 |
C2—C3—H3 | 120.3 | C11—C14—H14 | 119.1 |
C4—C3—H3 | 120.3 | O4'—C14—H14' | 117.7 |
C5—C4—C3 | 118.0 (4) | C11—C14—H14' | 117.7 |
O1Wi—Cd1—N2—C1 | 137.5 (4) | C5—C4—C6—O1 | 173.3 (11) |
O1W—Cd1—N2—C1 | −42.5 (4) | C3—C4—C6—O1 | −8.3 (13) |
O2W—Cd1—N2—C1 | −136.8 (4) | C5—C4—C6—O1' | −31.8 (11) |
O2Wi—Cd1—N2—C1 | 43.2 (4) | C3—C4—C6—O1' | 146.6 (9) |
O1Wi—Cd1—N2—C5 | −49.1 (4) | O2—C7—C8—C9 | 168.4 (5) |
O1W—Cd1—N2—C5 | 130.9 (4) | O3—C7—C8—C9 | −10.6 (7) |
O2W—Cd1—N2—C5 | 36.6 (4) | O2—C7—C8—C13 | −10.9 (8) |
O2Wi—Cd1—N2—C5 | −143.4 (4) | O3—C7—C8—C13 | 170.1 (5) |
C5—N2—C1—C2 | −1.8 (8) | C13—C8—C9—C10 | 1.2 (8) |
Cd1—N2—C1—C2 | 171.7 (4) | C7—C8—C9—C10 | −178.1 (5) |
N2—C1—C2—C3 | 2.5 (8) | C8—C9—C10—C11 | −3.4 (8) |
C1—C2—C3—C4 | −1.5 (8) | C9—C10—C11—C12 | 2.9 (8) |
C2—C3—C4—C5 | 0.0 (8) | C9—C10—C11—C14 | −178.3 (5) |
C2—C3—C4—C6 | −178.5 (5) | C10—C11—C12—C13 | −0.1 (8) |
C1—N2—C5—C4 | 0.1 (7) | C14—C11—C12—C13 | −179.0 (5) |
Cd1—N2—C5—C4 | −173.5 (4) | C11—C12—C13—C8 | −2.1 (8) |
C3—C4—C5—N2 | 0.7 (8) | C9—C8—C13—C12 | 1.6 (8) |
C6—C4—C5—N2 | 179.2 (5) | C7—C8—C13—C12 | −179.1 (5) |
C5—C4—C6—N1' | 151.4 (18) | C10—C11—C14—O4 | 176.8 (8) |
C3—C4—C6—N1' | −30.1 (19) | C12—C11—C14—O4 | −4.4 (11) |
C5—C4—C6—N1 | −0.7 (11) | C10—C11—C14—O4' | 0.1 (11) |
C3—C4—C6—N1 | 177.7 (9) | C12—C11—C14—O4' | 178.9 (8) |
Symmetry code: (i) −x+1, −y+1, −z+1. |
D—H···A | D—H | H···A | D···A | D—H···A |
O1W—H1W1···O2 | 0.85 (1) | 1.88 (2) | 2.715 (6) | 168 (6) |
O1W—H1W2···O3ii | 0.85 (1) | 1.98 (1) | 2.828 (6) | 172 (6) |
O2W—H2W1···O3i | 0.85 (1) | 2.02 (1) | 2.871 (6) | 178 (7) |
O2W—H2W2···O3iii | 0.85 (1) | 1.93 (1) | 2.782 (6) | 174 (7) |
N1—H1N1···O4iv | 0.86 | 2.03 | 2.86 (2) | 163 |
N1′—H1N3···O4′iv | 0.86 | 2.10 | 2.95 (4) | 173 |
Symmetry codes: (i) −x+1, −y+1, −z+1; (ii) −x+1, y+1/2, −z+1/2; (iii) x, −y+3/2, z+1/2; (iv) x+1, y, z+1. |
Experimental details
Crystal data | |
Chemical formula | [Cd(C6H6N2O)2(H2O)4](C8H5O3)2 |
Mr | 726.96 |
Crystal system, space group | Monoclinic, P21/c |
Temperature (K) | 295 |
a, b, c (Å) | 14.922 (1), 7.0382 (4), 14.030 (1) |
β (°) | 98.634 (2) |
V (Å3) | 1456.8 (2) |
Z | 2 |
Radiation type | Mo Kα |
µ (mm−1) | 0.82 |
Crystal size (mm) | 0.35 × 0.24 × 0.18 |
Data collection | |
Diffractometer | Rigaku R-AXIS RAPID IP |
Absorption correction | Multi-scan (ABSCOR; Higashi, 1995) |
Tmin, Tmax | 0.680, 0.866 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 13559, 3332, 2816 |
Rint | 0.035 |
(sin θ/λ)max (Å−1) | 0.649 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.048, 0.151, 1.14 |
No. of reflections | 3332 |
No. of parameters | 249 |
No. of restraints | 6 |
H-atom treatment | H atoms treated by a mixture of independent and constrained refinement |
Δρmax, Δρmin (e Å−3) | 1.08, −0.46 |
Computer programs: RAPID-AUTO (Rigaku, 1998), RAPID-AUTO, CrystalStructure (Rigaku/MSC, 2002), SHELXS97 (Sheldrick, 1997), SHELXL97 (Sheldrick, 1997), X-SEED (Barbour, 2001), publCIF (Westrip, 2007).
D—H···A | D—H | H···A | D···A | D—H···A |
O1W—H1W1···O2 | 0.85 (1) | 1.88 (2) | 2.715 (6) | 168 (6) |
O1W—H1W2···O3i | 0.85 (1) | 1.98 (1) | 2.828 (6) | 172 (6) |
O2W—H2W1···O3ii | 0.85 (1) | 2.02 (1) | 2.871 (6) | 178 (7) |
O2W—H2W2···O3iii | 0.85 (1) | 1.93 (1) | 2.782 (6) | 174 (7) |
N1—H1N1···O4iv | 0.86 | 2.03 | 2.86 (2) | 163 |
N1'—H1N3···O4'iv | 0.86 | 2.10 | 2.95 (4) | 173 |
Symmetry codes: (i) −x+1, y+1/2, −z+1/2; (ii) −x+1, −y+1, −z+1; (iii) x, −y+3/2, z+1/2; (iv) x+1, y, z+1. |
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Cadmium bis(4-formylbenzoate) forms a hydrated 1:2 adduct with imidazole; in the crystal structure, two molecules are linked by two Cd—Ocarboxyl interactions into a dinuclear species. The formylbenzoate anion functions in a chelating mode (Deng et al., 2006a). With the larger benzimidazole ligand, a 1:1 aqua adduct is formed, and one carboxylate anion is bidentate whereas the other is monodentate in the seven-coordinate structure (Deng et al., 2006b). Replacing the N-heterocycle by nicotinamide furnishes the title compound as a salt whose cation has two nicotinamide ligands binding to the tetraaquacadmium group; the carboxylate group is displaced from the coordination sphere and it exists as a free anion (Fig. 1). Hydrogen bonds link the cation and anion into a three-dimensional network.