Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536805029533/cv6578sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536805029533/cv6578Isup2.hkl |
CCDC reference: 287543
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (C-C) = 0.005 Å
- R factor = 0.027
- wR factor = 0.068
- Data-to-parameter ratio = 13.9
checkCIF/PLATON results
No syntax errors found
Alert level B PLAT232_ALERT_2_B Hirshfeld Test Diff (M-X) Cd1 - O2 .. 15.05 su PLAT232_ALERT_2_B Hirshfeld Test Diff (M-X) Cd1 - O3 .. 19.90 su
Alert level C PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT125_ALERT_4_C No _symmetry_space_group_name_Hall Given ....... ? PLAT199_ALERT_1_C Check the Reported _cell_measurement_temperature 293 K PLAT200_ALERT_1_C Check the Reported _diffrn_ambient_temperature . 293 K PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Cd1 - O4 .. 7.79 su PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for O3 PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for O4 PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for N3 PLAT380_ALERT_4_C Check Incorrectly? Oriented X(sp2)-Methyl Moiety C14 PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 52 O1W -CD1 -C15 -C16 142.60 1.60 1.555 1.555 1.555 1.555 PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 53 O4 -CD1 -C15 -C16 52.40 1.50 1.555 1.555 1.555 1.555 PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 54 N1 -CD1 -C15 -C16 -107.50 1.60 1.555 1.555 1.555 1.555 PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 55 N2 -CD1 -C15 -C16 -31.90 1.60 1.555 1.555 1.555 1.555 PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 56 O2 -CD1 -C15 -C16 64.20 1.60 1.555 1.555 1.555 1.555 PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 57 O5 -CD1 -C15 -C16 -132.10 1.70 1.555 1.555 1.555 1.555 PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 58 O3 -CD1 -C15 -C16 53.60 1.70 1.555 1.555 1.555 1.555 PLAT710_ALERT_4_C Delete 1-2-3 or 2-3-4 Linear Torsion Angle ... # 92 CD1 -C15 -C16 -C17 115.70 1.50 1.555 1.555 1.555 1.555 PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 4
0 ALERT level A = In general: serious problem 2 ALERT level B = Potentially serious problem 18 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 3 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 6 ALERT type 2 Indicator that the structure model may be wrong or deficient 0 ALERT type 3 Indicator that the structure quality may be low 11 ALERT type 4 Improvement, methodology, query or suggestion
To a solution of 2,9-dimethyl-1,10-phenanthroline (0.21 g, 1 mmol) and adipic acid (0.73 g, 0.5 mmol) in ethanol (10 ml) was added a solution of cadmium nitrate (0.31 g, 1 mmol) in distilled water (10 ml). The mixture was stirred and refluxed for 2 h. The hot solution was then filtered into another flask containing ethanol (10 ml). Orange crystals appeared over a period of one week by slow evaporation at room temperature.
C-bound H atoms were positioned geometrically and allowed to ride on their parent atoms, with C—H = 0.93–0.97 Å and Uiso(H) = 1.2–1.5Ueq(parent atom). The H atoms of the water molecules were located in a difference Fourier map and refined isotropically.
Data collection: SMART (Siemens, 1996); cell refinement: SAINT (Siemens, 1996); data reduction: SAINT; program(s) used to solve structure: SHELXTL (Sheldrick, 1997); program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL, PARST (Nardelli, 1995) and PLATON (Spek, 2003).
[Cd2(C6H8O4)(NO3)2(C14H12N2)2(H2O)2] | F(000) = 1976 |
Mr = 981.54 | Dx = 1.724 Mg m−3 |
Monoclinic, C2/c | Mo Kα radiation, λ = 0.71073 Å |
a = 24.438 (2) Å | Cell parameters from 5950 reflections |
b = 11.2315 (10) Å | θ = 2.4–26.1° |
c = 13.8799 (12) Å | µ = 1.20 mm−1 |
β = 96.969 (1)° | T = 293 K |
V = 3781.6 (6) Å3 | Column, orange |
Z = 4 | 0.30 × 0.16 × 0.07 mm |
Siemens SMART 1000 CCD area-detector diffractometer | 3730 independent reflections |
Radiation source: fine-focus sealed tube | 3367 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.016 |
Detector resolution: 8.33 pixels mm-1 | θmax = 26.1°, θmin = 1.7° |
ω scans | h = −26→30 |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | k = −8→13 |
Tmin = 0.715, Tmax = 0.921 | l = −17→16 |
10344 measured reflections |
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)] = 0.027 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.068 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.05 | w = 1/[σ2(Fo2) + (0.0341P)2 + 4.9157P] where P = (Fo2 + 2Fc2)/3 |
3730 reflections | (Δ/σ)max = 0.001 |
269 parameters | Δρmax = 0.48 e Å−3 |
0 restraints | Δρmin = −0.29 e Å−3 |
[Cd2(C6H8O4)(NO3)2(C14H12N2)2(H2O)2] | V = 3781.6 (6) Å3 |
Mr = 981.54 | Z = 4 |
Monoclinic, C2/c | Mo Kα radiation |
a = 24.438 (2) Å | µ = 1.20 mm−1 |
b = 11.2315 (10) Å | T = 293 K |
c = 13.8799 (12) Å | 0.30 × 0.16 × 0.07 mm |
β = 96.969 (1)° |
Siemens SMART 1000 CCD area-detector diffractometer | 3730 independent reflections |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | 3367 reflections with I > 2σ(I) |
Tmin = 0.715, Tmax = 0.921 | Rint = 0.016 |
10344 measured reflections |
R[F2 > 2σ(F2)] = 0.027 | 0 restraints |
wR(F2) = 0.068 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.05 | Δρmax = 0.48 e Å−3 |
3730 reflections | Δρmin = −0.29 e Å−3 |
269 parameters |
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. |
x | y | z | Uiso*/Ueq | ||
Cd1 | 0.350986 (7) | 0.222427 (17) | 0.404857 (12) | 0.03725 (8) | |
O5 | 0.31775 (7) | 0.16749 (18) | 0.23561 (12) | 0.0457 (4) | |
N1 | 0.43205 (8) | 0.1215 (2) | 0.38421 (14) | 0.0394 (5) | |
O1W | 0.28862 (10) | 0.0892 (2) | 0.45124 (18) | 0.0545 (5) | |
O4 | 0.28045 (9) | 0.3150 (2) | 0.30520 (14) | 0.0588 (5) | |
C4 | 0.52960 (11) | 0.1474 (4) | 0.37510 (18) | 0.0549 (8) | |
O3 | 0.39925 (10) | 0.2337 (2) | 0.58077 (18) | 0.0686 (6) | |
N3 | 0.36264 (12) | 0.2990 (2) | 0.60722 (18) | 0.0570 (7) | |
C15 | 0.28502 (11) | 0.2523 (2) | 0.23148 (19) | 0.0414 (6) | |
N2 | 0.41812 (9) | 0.3679 (2) | 0.38743 (14) | 0.0434 (5) | |
O2 | 0.32299 (9) | 0.3256 (2) | 0.54418 (15) | 0.0622 (5) | |
C7 | 0.51523 (13) | 0.3962 (3) | 0.3747 (2) | 0.0586 (9) | |
C12 | 0.47638 (10) | 0.1941 (3) | 0.38105 (17) | 0.0432 (6) | |
C16 | 0.25123 (13) | 0.2861 (3) | 0.1378 (2) | 0.0590 (8) | |
H16A | 0.2526 | 0.3720 | 0.1314 | 0.071* | |
H16B | 0.2132 | 0.2646 | 0.1425 | 0.071* | |
C5 | 0.57482 (13) | 0.2254 (4) | 0.3691 (2) | 0.0708 (11) | |
H5A | 0.6097 | 0.1937 | 0.3657 | 0.085* | |
C17 | 0.26777 (13) | 0.2313 (3) | 0.0458 (2) | 0.0532 (7) | |
H17A | 0.3057 | 0.2529 | 0.0403 | 0.080* | |
H17B | 0.2662 | 0.1453 | 0.0514 | 0.080* | |
C1 | 0.43836 (12) | 0.0037 (3) | 0.37968 (18) | 0.0475 (7) | |
C11 | 0.46922 (11) | 0.3224 (3) | 0.38166 (17) | 0.0445 (6) | |
C13 | 0.38890 (13) | −0.0733 (3) | 0.3787 (2) | 0.0590 (8) | |
H13A | 0.3569 | −0.0245 | 0.3815 | 0.089* | |
H13B | 0.3934 | −0.1256 | 0.4338 | 0.089* | |
H13C | 0.3844 | −0.1197 | 0.3202 | 0.089* | |
C9 | 0.45471 (17) | 0.5631 (3) | 0.3769 (2) | 0.0700 (10) | |
H9A | 0.4488 | 0.6449 | 0.3745 | 0.084* | |
C10 | 0.41070 (13) | 0.4858 (3) | 0.3856 (2) | 0.0534 (7) | |
C2 | 0.49046 (13) | −0.0473 (3) | 0.3751 (2) | 0.0591 (8) | |
H2A | 0.4941 | −0.1297 | 0.3733 | 0.071* | |
C8 | 0.50601 (16) | 0.5191 (4) | 0.3720 (2) | 0.0726 (11) | |
H8A | 0.5352 | 0.5710 | 0.3668 | 0.087* | |
O1 | 0.36506 (14) | 0.3354 (4) | 0.68990 (19) | 0.1108 (11) | |
C3 | 0.53512 (13) | 0.0224 (4) | 0.3732 (2) | 0.0625 (9) | |
H3A | 0.5696 | −0.0117 | 0.3707 | 0.075* | |
O2W | 0.30667 (11) | 0.0534 (3) | 0.64346 (18) | 0.0644 (6) | |
C14 | 0.35495 (14) | 0.5343 (3) | 0.3939 (2) | 0.0643 (9) | |
H14A | 0.3298 | 0.4698 | 0.3996 | 0.096* | |
H14B | 0.3426 | 0.5802 | 0.3370 | 0.096* | |
H14C | 0.3564 | 0.5842 | 0.4503 | 0.096* | |
C6 | 0.56816 (13) | 0.3436 (5) | 0.3684 (2) | 0.0716 (11) | |
H6A | 0.5984 | 0.3926 | 0.3638 | 0.086* | |
H2W1 | 0.2546 (18) | 0.110 (4) | 0.435 (3) | 0.098 (15)* | |
H2W2 | 0.3072 (15) | −0.010 (4) | 0.670 (3) | 0.077 (13)* | |
H1W1 | 0.2946 (15) | 0.076 (4) | 0.509 (3) | 0.078 (13)* | |
H1W2 | 0.279 (2) | 0.099 (5) | 0.661 (4) | 0.14 (2)* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Cd1 | 0.03456 (12) | 0.04430 (13) | 0.03231 (11) | 0.00217 (8) | 0.00174 (7) | 0.00127 (7) |
O5 | 0.0458 (10) | 0.0537 (12) | 0.0356 (9) | 0.0082 (9) | −0.0034 (7) | −0.0006 (8) |
N1 | 0.0361 (11) | 0.0513 (13) | 0.0294 (10) | 0.0051 (10) | −0.0013 (8) | −0.0002 (9) |
O1W | 0.0546 (13) | 0.0576 (13) | 0.0533 (13) | −0.0033 (11) | 0.0149 (10) | 0.0048 (11) |
O4 | 0.0714 (14) | 0.0598 (13) | 0.0416 (11) | 0.0192 (11) | −0.0073 (9) | −0.0082 (10) |
C4 | 0.0363 (14) | 0.099 (3) | 0.0283 (12) | 0.0034 (15) | −0.0004 (10) | −0.0023 (14) |
O3 | 0.0562 (14) | 0.0897 (18) | 0.0601 (14) | 0.0053 (12) | 0.0082 (11) | 0.0096 (12) |
N3 | 0.0638 (17) | 0.0648 (17) | 0.0424 (14) | −0.0182 (14) | 0.0070 (12) | −0.0122 (12) |
C15 | 0.0430 (14) | 0.0483 (16) | 0.0308 (13) | −0.0018 (12) | −0.0043 (11) | 0.0009 (11) |
N2 | 0.0490 (13) | 0.0488 (13) | 0.0316 (10) | −0.0062 (10) | 0.0016 (9) | 0.0029 (9) |
O2 | 0.0574 (13) | 0.0775 (15) | 0.0522 (12) | 0.0063 (12) | 0.0084 (10) | 0.0018 (11) |
C7 | 0.0547 (18) | 0.088 (3) | 0.0321 (14) | −0.0268 (17) | 0.0001 (12) | 0.0023 (14) |
C12 | 0.0367 (13) | 0.0690 (19) | 0.0228 (11) | −0.0001 (12) | −0.0002 (9) | −0.0008 (11) |
C16 | 0.0567 (18) | 0.071 (2) | 0.0446 (16) | 0.0185 (16) | −0.0112 (14) | −0.0052 (14) |
C5 | 0.0344 (16) | 0.136 (4) | 0.0418 (17) | −0.0040 (19) | 0.0030 (12) | −0.004 (2) |
C17 | 0.0523 (17) | 0.067 (2) | 0.0370 (15) | 0.0106 (14) | −0.0063 (13) | 0.0024 (13) |
C1 | 0.0507 (15) | 0.0567 (18) | 0.0330 (13) | 0.0138 (14) | −0.0034 (11) | −0.0022 (12) |
C11 | 0.0416 (14) | 0.0675 (18) | 0.0235 (11) | −0.0105 (13) | 0.0005 (10) | 0.0019 (12) |
C13 | 0.0609 (18) | 0.0466 (17) | 0.0671 (19) | 0.0056 (15) | −0.0024 (15) | −0.0007 (15) |
C9 | 0.095 (3) | 0.057 (2) | 0.0560 (19) | −0.025 (2) | 0.0030 (18) | 0.0066 (16) |
C10 | 0.072 (2) | 0.0504 (17) | 0.0372 (14) | −0.0129 (15) | 0.0016 (13) | 0.0045 (12) |
C2 | 0.0579 (19) | 0.071 (2) | 0.0459 (16) | 0.0255 (17) | −0.0014 (13) | −0.0061 (15) |
C8 | 0.083 (3) | 0.086 (3) | 0.0472 (17) | −0.046 (2) | 0.0008 (16) | 0.0069 (17) |
O1 | 0.131 (3) | 0.150 (3) | 0.0516 (15) | −0.022 (2) | 0.0094 (15) | −0.0447 (18) |
C3 | 0.0464 (17) | 0.100 (3) | 0.0399 (15) | 0.0270 (18) | 0.0022 (12) | −0.0072 (16) |
O2W | 0.0801 (17) | 0.0564 (15) | 0.0588 (14) | 0.0042 (13) | 0.0162 (12) | 0.0120 (12) |
C14 | 0.087 (2) | 0.0419 (17) | 0.064 (2) | 0.0046 (16) | 0.0087 (18) | 0.0033 (14) |
C6 | 0.0449 (18) | 0.127 (4) | 0.0418 (16) | −0.031 (2) | 0.0023 (13) | 0.003 (2) |
Cd1—O1W | 2.283 (2) | C16—C17 | 1.516 (4) |
Cd1—O4 | 2.321 (2) | C16—H16A | 0.9700 |
Cd1—N1 | 2.330 (2) | C16—H16B | 0.9700 |
Cd1—N2 | 2.348 (2) | C5—C6 | 1.338 (6) |
Cd1—O2 | 2.423 (2) | C5—H5A | 0.9300 |
Cd1—O5 | 2.4690 (17) | C17—C17i | 1.511 (5) |
Cd1—O3 | 2.583 (3) | C17—H17A | 0.9700 |
Cd1—C15 | 2.750 (3) | C17—H17B | 0.9700 |
O5—C15 | 1.240 (3) | C1—C2 | 1.405 (4) |
N1—C1 | 1.335 (4) | C1—C13 | 1.485 (4) |
N1—C12 | 1.361 (3) | C13—H13A | 0.9600 |
O1W—H2W1 | 0.87 (4) | C13—H13B | 0.9600 |
O1W—H1W1 | 0.81 (4) | C13—H13C | 0.9600 |
O4—C15 | 1.258 (3) | C9—C8 | 1.357 (5) |
C4—C3 | 1.411 (5) | C9—C10 | 1.399 (4) |
C4—C12 | 1.414 (4) | C9—H9A | 0.9300 |
C4—C5 | 1.420 (5) | C10—C14 | 1.484 (4) |
O3—N3 | 1.247 (4) | C2—C3 | 1.346 (5) |
N3—O1 | 1.213 (3) | C2—H2A | 0.9300 |
N3—O2 | 1.260 (3) | C8—H8A | 0.9300 |
C15—C16 | 1.502 (4) | C3—H3A | 0.9300 |
N2—C10 | 1.337 (4) | O2W—H2W2 | 0.80 (4) |
N2—C11 | 1.361 (4) | O2W—H1W2 | 0.90 (6) |
C7—C8 | 1.398 (5) | C14—H14A | 0.9600 |
C7—C11 | 1.410 (4) | C14—H14B | 0.9600 |
C7—C6 | 1.434 (5) | C14—H14C | 0.9600 |
C12—C11 | 1.452 (4) | C6—H6A | 0.9300 |
O1W—Cd1—O4 | 89.34 (9) | N1—C12—C4 | 121.4 (3) |
O1W—Cd1—N1 | 108.81 (8) | N1—C12—C11 | 119.8 (2) |
O4—Cd1—N1 | 136.52 (7) | C4—C12—C11 | 118.7 (3) |
O1W—Cd1—N2 | 169.53 (8) | C15—C16—C17 | 116.8 (2) |
O4—Cd1—N2 | 96.01 (8) | C15—C16—H16A | 108.1 |
N1—Cd1—N2 | 73.19 (8) | C17—C16—H16A | 108.1 |
O1W—Cd1—O2 | 79.95 (8) | C15—C16—H16B | 108.1 |
O4—Cd1—O2 | 90.02 (7) | C17—C16—H16B | 108.1 |
N1—Cd1—O2 | 131.10 (7) | H16A—C16—H16B | 107.3 |
N2—Cd1—O2 | 91.03 (8) | C6—C5—C4 | 121.2 (3) |
O1W—Cd1—O5 | 87.17 (8) | C6—C5—H5A | 119.4 |
O4—Cd1—O5 | 53.84 (7) | C4—C5—H5A | 119.4 |
N1—Cd1—O5 | 87.02 (6) | C17i—C17—C16 | 114.3 (3) |
N2—Cd1—O5 | 103.25 (7) | C17i—C17—H17A | 108.7 |
O2—Cd1—O5 | 141.87 (7) | C16—C17—H17A | 108.7 |
O1W—Cd1—O3 | 90.54 (9) | C17i—C17—H17B | 108.7 |
O4—Cd1—O3 | 139.69 (8) | C16—C17—H17B | 108.7 |
N1—Cd1—O3 | 80.93 (7) | H17A—C17—H17B | 107.6 |
N2—Cd1—O3 | 79.56 (7) | N1—C1—C2 | 121.1 (3) |
O2—Cd1—O3 | 50.43 (8) | N1—C1—C13 | 118.6 (2) |
O5—Cd1—O3 | 166.29 (7) | C2—C1—C13 | 120.2 (3) |
O1W—Cd1—C15 | 89.21 (9) | N2—C11—C7 | 121.9 (3) |
O4—Cd1—C15 | 27.08 (8) | N2—C11—C12 | 119.0 (2) |
N1—Cd1—C15 | 111.63 (8) | C7—C11—C12 | 119.1 (3) |
N2—Cd1—C15 | 99.66 (8) | C1—C13—H13A | 109.5 |
O2—Cd1—C15 | 116.61 (8) | C1—C13—H13B | 109.5 |
O5—Cd1—C15 | 26.81 (7) | H13A—C13—H13B | 109.5 |
O3—Cd1—C15 | 166.77 (8) | C1—C13—H13C | 109.5 |
C15—O5—Cd1 | 89.31 (15) | H13A—C13—H13C | 109.5 |
C1—N1—C12 | 119.7 (2) | H13B—C13—H13C | 109.5 |
C1—N1—Cd1 | 126.37 (18) | C8—C9—C10 | 120.2 (4) |
C12—N1—Cd1 | 113.87 (18) | C8—C9—H9A | 119.9 |
Cd1—O1W—H2W1 | 114 (3) | C10—C9—H9A | 119.9 |
Cd1—O1W—H1W1 | 111 (3) | N2—C10—C9 | 120.8 (3) |
H2W1—O1W—H1W1 | 111 (4) | N2—C10—C14 | 119.0 (3) |
C15—O4—Cd1 | 95.82 (17) | C9—C10—C14 | 120.1 (3) |
C3—C4—C12 | 117.4 (3) | C3—C2—C1 | 120.3 (3) |
C3—C4—C5 | 122.4 (3) | C3—C2—H2A | 119.8 |
C12—C4—C5 | 120.2 (3) | C1—C2—H2A | 119.8 |
N3—O3—Cd1 | 92.60 (17) | C9—C8—C7 | 120.3 (3) |
O1—N3—O3 | 121.5 (3) | C9—C8—H8A | 119.8 |
O1—N3—O2 | 121.5 (3) | C7—C8—H8A | 119.8 |
O3—N3—O2 | 117.0 (2) | C2—C3—C4 | 119.9 (3) |
O5—C15—O4 | 120.8 (2) | C2—C3—H3A | 120.0 |
O5—C15—C16 | 121.2 (2) | C4—C3—H3A | 120.0 |
O4—C15—C16 | 117.9 (3) | H2W2—O2W—H1W2 | 111 (4) |
O5—C15—Cd1 | 63.88 (13) | C10—C14—H14A | 109.5 |
O4—C15—Cd1 | 57.11 (13) | C10—C14—H14B | 109.5 |
C16—C15—Cd1 | 172.2 (2) | H14A—C14—H14B | 109.5 |
C10—N2—C11 | 119.6 (3) | C10—C14—H14C | 109.5 |
C10—N2—Cd1 | 126.6 (2) | H14A—C14—H14C | 109.5 |
C11—N2—Cd1 | 113.75 (19) | H14B—C14—H14C | 109.5 |
N3—O2—Cd1 | 99.97 (17) | C5—C6—C7 | 121.2 (3) |
C8—C7—C11 | 117.1 (3) | C5—C6—H6A | 119.4 |
C8—C7—C6 | 123.3 (3) | C7—C6—H6A | 119.4 |
C11—C7—C6 | 119.7 (4) | ||
O1W—Cd1—O5—C15 | 93.84 (17) | C15—Cd1—N2—C10 | 67.6 (2) |
O4—Cd1—O5—C15 | 2.58 (17) | O1W—Cd1—N2—C11 | 98.1 (5) |
N1—Cd1—O5—C15 | −157.15 (17) | O4—Cd1—N2—C11 | −141.40 (16) |
N2—Cd1—O5—C15 | −85.20 (17) | N1—Cd1—N2—C11 | −4.48 (16) |
O2—Cd1—O5—C15 | 24.1 (2) | O2—Cd1—N2—C11 | 128.47 (17) |
O3—Cd1—O5—C15 | 174.5 (3) | O5—Cd1—N2—C11 | −87.18 (16) |
O1W—Cd1—N1—C1 | 13.0 (2) | O3—Cd1—N2—C11 | 79.10 (17) |
O4—Cd1—N1—C1 | −97.0 (2) | C15—Cd1—N2—C11 | −114.31 (17) |
N2—Cd1—N1—C1 | −177.8 (2) | O1—N3—O2—Cd1 | 179.1 (3) |
O2—Cd1—N1—C1 | 106.0 (2) | O3—N3—O2—Cd1 | −0.9 (3) |
O5—Cd1—N1—C1 | −73.0 (2) | O1W—Cd1—O2—N3 | 99.65 (19) |
O3—Cd1—N1—C1 | 100.5 (2) | O4—Cd1—O2—N3 | −171.02 (19) |
C15—Cd1—N1—C1 | −83.9 (2) | N1—Cd1—O2—N3 | −6.6 (2) |
O1W—Cd1—N1—C12 | −164.07 (16) | N2—Cd1—O2—N3 | −75.00 (18) |
O4—Cd1—N1—C12 | 85.95 (19) | O5—Cd1—O2—N3 | 171.78 (15) |
N2—Cd1—N1—C12 | 5.14 (16) | O3—Cd1—O2—N3 | 0.52 (17) |
O2—Cd1—N1—C12 | −71.06 (19) | C15—Cd1—O2—N3 | −176.34 (17) |
O5—Cd1—N1—C12 | 109.94 (16) | C1—N1—C12—C4 | −1.4 (3) |
O3—Cd1—N1—C12 | −76.61 (16) | Cd1—N1—C12—C4 | 175.92 (18) |
C15—Cd1—N1—C12 | 99.08 (17) | C1—N1—C12—C11 | 177.3 (2) |
O1W—Cd1—O4—C15 | −89.54 (19) | Cd1—N1—C12—C11 | −5.4 (3) |
N1—Cd1—O4—C15 | 27.6 (2) | C3—C4—C12—N1 | −0.4 (4) |
N2—Cd1—O4—C15 | 99.47 (19) | C5—C4—C12—N1 | 178.2 (2) |
O2—Cd1—O4—C15 | −169.49 (19) | C3—C4—C12—C11 | −179.1 (2) |
O5—Cd1—O4—C15 | −2.56 (16) | C5—C4—C12—C11 | −0.5 (4) |
O3—Cd1—O4—C15 | −179.59 (17) | O5—C15—C16—C17 | −13.2 (5) |
O1W—Cd1—O3—N3 | −76.98 (18) | O4—C15—C16—C17 | 164.6 (3) |
O4—Cd1—O3—N3 | 12.6 (2) | Cd1—C15—C16—C17 | 115.7 (15) |
N1—Cd1—O3—N3 | 174.05 (19) | C3—C4—C5—C6 | 178.2 (3) |
N2—Cd1—O3—N3 | 99.62 (19) | C12—C4—C5—C6 | −0.4 (4) |
O2—Cd1—O3—N3 | −0.52 (17) | C15—C16—C17—C17i | −180.0 (4) |
O5—Cd1—O3—N3 | −157.2 (3) | C12—N1—C1—C2 | 2.2 (4) |
C15—Cd1—O3—N3 | 11.8 (5) | Cd1—N1—C1—C2 | −174.68 (19) |
Cd1—O3—N3—O1 | −179.2 (3) | C12—N1—C1—C13 | −177.2 (2) |
Cd1—O3—N3—O2 | 0.9 (3) | Cd1—N1—C1—C13 | 5.9 (3) |
Cd1—O5—C15—O4 | −4.5 (3) | C10—N2—C11—C7 | 0.6 (4) |
Cd1—O5—C15—C16 | 173.2 (3) | Cd1—N2—C11—C7 | −177.59 (18) |
Cd1—O4—C15—O5 | 4.8 (3) | C10—N2—C11—C12 | −178.3 (2) |
Cd1—O4—C15—C16 | −173.0 (2) | Cd1—N2—C11—C12 | 3.5 (3) |
O1W—Cd1—C15—O5 | −85.30 (17) | C8—C7—C11—N2 | −1.2 (4) |
O4—Cd1—C15—O5 | −175.4 (3) | C6—C7—C11—N2 | −179.8 (2) |
N1—Cd1—C15—O5 | 24.66 (18) | C8—C7—C11—C12 | 177.8 (2) |
N2—Cd1—C15—O5 | 100.29 (17) | C6—C7—C11—C12 | −0.8 (4) |
O2—Cd1—C15—O5 | −163.65 (15) | N1—C12—C11—N2 | 1.3 (3) |
O3—Cd1—C15—O5 | −174.3 (3) | C4—C12—C11—N2 | −180.0 (2) |
O1W—Cd1—C15—O4 | 90.11 (19) | N1—C12—C11—C7 | −177.6 (2) |
N1—Cd1—C15—O4 | −159.92 (18) | C4—C12—C11—C7 | 1.1 (3) |
N2—Cd1—C15—O4 | −84.29 (19) | C11—N2—C10—C9 | 0.6 (4) |
O2—Cd1—C15—O4 | 11.8 (2) | Cd1—N2—C10—C9 | 178.6 (2) |
O5—Cd1—C15—O4 | 175.4 (3) | C11—N2—C10—C14 | −178.8 (2) |
O3—Cd1—C15—O4 | 1.2 (5) | Cd1—N2—C10—C14 | −0.9 (4) |
O1W—Cd1—C15—C16 | 142.6 (16) | C8—C9—C10—N2 | −1.2 (5) |
O4—Cd1—C15—C16 | 52.4 (15) | C8—C9—C10—C14 | 178.2 (3) |
N1—Cd1—C15—C16 | −107.5 (16) | N1—C1—C2—C3 | −1.3 (4) |
N2—Cd1—C15—C16 | −31.9 (16) | C13—C1—C2—C3 | 178.1 (3) |
O2—Cd1—C15—C16 | 64.2 (16) | C10—C9—C8—C7 | 0.6 (5) |
O5—Cd1—C15—C16 | −132.1 (17) | C11—C7—C8—C9 | 0.6 (4) |
O3—Cd1—C15—C16 | 53.6 (17) | C6—C7—C8—C9 | 179.1 (3) |
O1W—Cd1—N2—C10 | −79.9 (5) | C1—C2—C3—C4 | −0.5 (4) |
O4—Cd1—N2—C10 | 40.5 (2) | C12—C4—C3—C2 | 1.3 (4) |
N1—Cd1—N2—C10 | 177.4 (2) | C5—C4—C3—C2 | −177.3 (3) |
O2—Cd1—N2—C10 | −49.6 (2) | C4—C5—C6—C7 | 0.7 (5) |
O5—Cd1—N2—C10 | 94.7 (2) | C8—C7—C6—C5 | −178.5 (3) |
O3—Cd1—N2—C10 | −99.0 (2) | C11—C7—C6—C5 | 0.0 (4) |
Symmetry code: (i) −x+1/2, −y+1/2, −z. |
D—H···A | D—H | H···A | D···A | D—H···A |
O1W—H1W1···O2W | 0.81 (4) | 1.87 (4) | 2.681 (4) | 177 (4) |
O2W—H1W2···O4ii | 0.90 (5) | 1.85 (5) | 2.756 (4) | 177 (5) |
O2W—H2W2···O5iii | 0.80 (4) | 1.99 (4) | 2.789 (4) | 173 (4) |
C14—H14B···O1iv | 0.96 | 2.37 | 3.223 (4) | 147 |
Symmetry codes: (ii) −x+1/2, −y+1/2, −z+1; (iii) x, −y, z+1/2; (iv) x, −y+1, z−1/2. |
Experimental details
Crystal data | |
Chemical formula | [Cd2(C6H8O4)(NO3)2(C14H12N2)2(H2O)2] |
Mr | 981.54 |
Crystal system, space group | Monoclinic, C2/c |
Temperature (K) | 293 |
a, b, c (Å) | 24.438 (2), 11.2315 (10), 13.8799 (12) |
β (°) | 96.969 (1) |
V (Å3) | 3781.6 (6) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 1.20 |
Crystal size (mm) | 0.30 × 0.16 × 0.07 |
Data collection | |
Diffractometer | Siemens SMART 1000 CCD area-detector diffractometer |
Absorption correction | Multi-scan (SADABS; Sheldrick, 1996) |
Tmin, Tmax | 0.715, 0.921 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 10344, 3730, 3367 |
Rint | 0.016 |
(sin θ/λ)max (Å−1) | 0.618 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.027, 0.068, 1.05 |
No. of reflections | 3730 |
No. of parameters | 269 |
H-atom treatment | H atoms treated by a mixture of independent and constrained refinement |
Δρmax, Δρmin (e Å−3) | 0.48, −0.29 |
Computer programs: SMART (Siemens, 1996), SAINT (Siemens, 1996), SAINT, SHELXTL (Sheldrick, 1997), SHELXTL, PARST (Nardelli, 1995) and PLATON (Spek, 2003).
Cd1—O1W | 2.283 (2) | Cd1—O2 | 2.423 (2) |
Cd1—O4 | 2.321 (2) | Cd1—O5 | 2.4690 (17) |
Cd1—N1 | 2.330 (2) | Cd1—O3 | 2.583 (3) |
Cd1—N2 | 2.348 (2) |
D—H···A | D—H | H···A | D···A | D—H···A |
O1W—H1W1···O2W | 0.81 (4) | 1.87 (4) | 2.681 (4) | 177 (4) |
O2W—H1W2···O4i | 0.90 (5) | 1.85 (5) | 2.756 (4) | 177 (5) |
O2W—H2W2···O5ii | 0.80 (4) | 1.99 (4) | 2.789 (4) | 173 (4) |
C14—H14B···O1iii | 0.96 | 2.37 | 3.223 (4) | 147 |
Symmetry codes: (i) −x+1/2, −y+1/2, −z+1; (ii) x, −y, z+1/2; (iii) x, −y+1, z−1/2. |
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Recently, we reported the structure of di-µ-adipato-κ6O,O':O'';O:O',O''-bis[aqua(1,10-phenanthroline-κ2N,N)zinc(II)] (Ding et al., 2005). In our ongoing studies, we synthesized the title compound, (I). An X-ray crystallographic analysis was undertaken to determine the stereochemistry of (I).
The binuclear cadmium complex molecule in (I) possesses a crystallographically imposed centre of symmetry (Fig. 1). Each CdII atom is seven-coordinated by two N atoms and five O atoms (Table 1) in a distorted petagonal–bipyramidal geometry. One axial position is occupied by atom O1W of the water molecule, with a Cd—O distance of 2.283 (2) Å. The other axial position is occupied by atom N2 of the 2,9-dimethylphenanthroline ligand.
In the crystal structure, the water molecules act as both donors and acceptors to form O—H···O hydrogen bonds (Table 2). These hydrogen bonds link the molecules into double chains along the c axis (Fig. 2). The short Cg1···Cg1i distance of 3.508 (2) Å [Cg1 is the centroid of the C4–C7/C11/C12 ring; symmetry code: (i) 1 − x, y, 1/2 − z] indicates an existence of π–π stacking interactions between the tricycles, which stabilize the packing.