The title compound, {[Cd(C
6H
16N
2)(H
2O)
4](C
8H
4O
4)·2H
2O}
n, (I), exhibits a chain structure. The central Cd
II ion is coordinated by four water molecules and two N atoms derived from two 1,6-diaminohexane molecules, giving a zigzag-shaped polymeric chain with a [Cd—N—C—C—C—C—C—C—N]
n backbone running parallel to the
b axis. The two independent terephthalate anions are not coordinated to cadmium(II), acting rather as counter-ions. Each coordinated water molecule forms strong O—H
O hydrogen bonds with the adjacent terephthalate counter-ions, forming a three-dimensional hydrogen-bonded supramolecular architecture.
Supporting information
CCDC reference: 263540
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (C-C) = 0.005 Å
- R factor = 0.036
- wR factor = 0.084
- Data-to-parameter ratio = 12.7
checkCIF/PLATON results
No syntax errors found
Alert level C
PLAT199_ALERT_1_C Check the Reported cell_measurement_temperature 293
PLAT200_ALERT_1_C Check the Reported cell_ambient_temperature .... 293
PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for Cd1
PLAT731_ALERT_1_C Bond Calc 0.87(4), Rep 0.872(19) ...... 2.11 su-Rat
O3 -H11 1.555 1.555
PLAT731_ALERT_1_C Bond Calc 0.91(4), Rep 0.909(19) ...... 2.11 su-Rat
O5 -H12 1.555 1.555
PLAT731_ALERT_1_C Bond Calc 0.92(4), Rep 0.920(19) ...... 2.11 su-Rat
O6 -H13 1.555 1.555
PLAT735_ALERT_1_C D-H Calc 0.87(4), Rep 0.872(19) ...... 2.11 su-Rat
O3 -H11 1.555 1.555
PLAT735_ALERT_1_C D-H Calc 0.91(4), Rep 0.909(19) ...... 2.11 su-Rat
O5 -H12 1.555 1.555
PLAT735_ALERT_1_C D-H Calc 0.92(4), Rep 0.920(19) ...... 2.11 su-Rat
O6 -H13 1.555 1.555
0 ALERT level A = In general: serious problem
0 ALERT level B = Potentially serious problem
9 ALERT level C = Check and explain
0 ALERT level G = General alerts; check
8 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
1 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
0 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: SMART (Siemens, 1996); cell refinement: SMART; data reduction: SAINT (Siemens, 1996); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997a); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997a); molecular graphics: SHELXTL (Sheldrick, 1997b); software used to prepare material for publication: SHELXTL.
catena-Poly [tetraqua cadmium(II)-µ-hexane-1,6-diamineK
2N:
N']
terephthalate dihydrate]
top
Crystal data top
[Cd(C6H16N2)(H2O)4](C8H4O4).2H2O | F(000) = 516 |
Mr = 500.82 | Dx = 1.517 Mg m−3 |
Monoclinic, P21/m | Melting point: 473 K |
Hall symbol: -P 2yb | Mo Kα radiation, λ = 0.71073 Å |
a = 6.4744 (16) Å | Cell parameters from 800 reflections |
b = 23.758 (6) Å | θ = 2.3–25.0° |
c = 7.5236 (19) Å | µ = 1.05 mm−1 |
β = 108.715 (3)° | T = 293 K |
V = 1096.1 (5) Å3 | Block, colorless |
Z = 2 | 0.45 × 0.38 × 0.30 mm |
Data collection top
Siemens SMART CCD area-detector diffractometer | 1949 independent reflections |
Radiation source: fine-focus sealed tube | 1886 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.027 |
Detector resolution: 0 pixels mm-1 | θmax = 25.0°, θmin = 2.9° |
φ and ω scans | h = −7→7 |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | k = −28→28 |
Tmin = 0.631, Tmax = 0.727 | l = −8→8 |
5584 measured reflections | |
Refinement top
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)] = 0.036 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.085 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.22 | w = 1/[σ2(Fo2) + (0.0278P)2 + 1.7591P] where P = (Fo2 + 2Fc2)/3 |
1949 reflections | (Δ/σ)max = 0.001 |
154 parameters | Δρmax = 0.77 e Å−3 |
4 restraints | Δρmin = −1.44 e Å−3 |
Special details top
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. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Cd1 | 0.62774 (6) | 0.7500 | 0.84776 (6) | 0.03019 (15) | |
N1 | 0.5885 (5) | 0.65322 (13) | 0.8507 (5) | 0.0351 (7) | |
H1 | 0.5269 | 0.6441 | 0.9384 | 0.042* | |
H2 | 0.4972 | 0.6421 | 0.7386 | 0.042* | |
O1 | 0.2193 (5) | 0.64059 (11) | 0.4697 (5) | 0.0466 (7) | |
O2 | −0.1387 (5) | 0.64981 (12) | 0.4028 (5) | 0.0530 (8) | |
O3 | 0.3448 (7) | 0.7500 | 1.0096 (6) | 0.0434 (10) | |
O4 | 0.3548 (7) | 0.7500 | 0.5539 (7) | 0.0496 (12) | |
O5 | 0.8842 (9) | 0.7500 | 0.6900 (8) | 0.0620 (13) | |
O6 | 0.8848 (8) | 0.7500 | 1.1526 (7) | 0.0559 (12) | |
O7 | 0.4300 (7) | 0.65045 (16) | 0.2033 (5) | 0.0577 (9) | |
C1 | 0.0315 (6) | 0.62079 (15) | 0.4452 (5) | 0.0319 (8) | |
C2 | 0.0140 (6) | 0.55813 (15) | 0.4724 (5) | 0.0284 (8) | |
C3 | −0.1863 (6) | 0.53291 (15) | 0.4497 (5) | 0.0332 (8) | |
H3 | −0.3125 | 0.5546 | 0.4152 | 0.040* | |
C4 | 0.1993 (6) | 0.52464 (15) | 0.5216 (5) | 0.0330 (8) | |
H4 | 0.3343 | 0.5409 | 0.5357 | 0.040* | |
C5 | 0.7966 (7) | 0.62221 (16) | 0.8898 (6) | 0.0406 (9) | |
H5 | 0.9040 | 0.6395 | 0.9968 | 0.049* | |
H6 | 0.8480 | 0.6262 | 0.7828 | 0.049* | |
C6 | 0.7832 (7) | 0.55990 (15) | 0.9302 (6) | 0.0383 (9) | |
H7 | 0.7263 | 0.5554 | 1.0340 | 0.046* | |
H8 | 0.6826 | 0.5418 | 0.8211 | 0.046* | |
C7 | 1.0038 (7) | 0.53129 (15) | 0.9786 (6) | 0.0401 (10) | |
H9 | 1.1043 | 0.5498 | 1.0869 | 0.048* | |
H10 | 1.0599 | 0.5358 | 0.8744 | 0.048* | |
H11 | 0.374 (9) | 0.7199 (15) | 1.079 (7) | 0.073 (18)* | |
H12 | 0.898 (9) | 0.7172 (14) | 0.633 (7) | 0.071 (17)* | |
H13 | 0.884 (8) | 0.7193 (14) | 1.227 (6) | 0.060 (15)* | |
H14 | 0.257 (5) | 0.7241 (14) | 0.518 (6) | 0.044 (13)* | |
H15 | 0.553 (10) | 0.647 (2) | 0.263 (8) | 0.061 (18)* | |
H16 | 0.355 (9) | 0.643 (2) | 0.283 (8) | 0.075 (18)* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Cd1 | 0.0286 (2) | 0.0214 (2) | 0.0359 (2) | 0.000 | 0.00379 (16) | 0.000 |
N1 | 0.0363 (18) | 0.0263 (15) | 0.0367 (17) | 0.0046 (13) | 0.0035 (14) | 0.0015 (13) |
O1 | 0.0446 (17) | 0.0277 (14) | 0.065 (2) | −0.0124 (13) | 0.0146 (15) | 0.0017 (13) |
O2 | 0.0443 (17) | 0.0282 (14) | 0.079 (2) | 0.0038 (13) | 0.0100 (16) | 0.0063 (15) |
O3 | 0.039 (2) | 0.041 (2) | 0.049 (3) | 0.000 | 0.012 (2) | 0.000 |
O4 | 0.042 (3) | 0.026 (2) | 0.057 (3) | 0.000 | −0.018 (2) | 0.000 |
O5 | 0.069 (3) | 0.050 (3) | 0.075 (4) | 0.000 | 0.034 (3) | 0.000 |
O6 | 0.066 (3) | 0.040 (2) | 0.048 (3) | 0.000 | −0.001 (2) | 0.000 |
O7 | 0.046 (2) | 0.069 (2) | 0.055 (2) | −0.0008 (18) | 0.0129 (19) | 0.0132 (18) |
C1 | 0.035 (2) | 0.0260 (18) | 0.030 (2) | −0.0029 (16) | 0.0036 (16) | −0.0006 (15) |
C2 | 0.0314 (19) | 0.0262 (17) | 0.0260 (18) | −0.0034 (15) | 0.0069 (15) | −0.0005 (14) |
C3 | 0.029 (2) | 0.0283 (18) | 0.040 (2) | 0.0014 (15) | 0.0090 (16) | 0.0029 (16) |
C4 | 0.0269 (19) | 0.0300 (19) | 0.040 (2) | −0.0071 (15) | 0.0081 (16) | 0.0017 (16) |
C5 | 0.040 (2) | 0.0288 (19) | 0.049 (2) | 0.0074 (17) | 0.0084 (19) | 0.0038 (17) |
C6 | 0.049 (2) | 0.0275 (19) | 0.033 (2) | 0.0111 (17) | 0.0058 (18) | 0.0042 (16) |
C7 | 0.053 (3) | 0.028 (2) | 0.036 (2) | 0.0123 (18) | 0.0085 (19) | 0.0047 (16) |
Geometric parameters (Å, º) top
Cd1—N1 | 2.314 (3) | C1—C2 | 1.512 (5) |
Cd1—N1i | 2.314 (3) | C2—C4 | 1.387 (5) |
Cd1—O5 | 2.330 (5) | C2—C3 | 1.388 (5) |
Cd1—O4 | 2.346 (4) | C3—C4ii | 1.391 (5) |
Cd1—O6 | 2.362 (5) | C3—H3 | 0.9300 |
Cd1—O3 | 2.504 (4) | C4—C3ii | 1.391 (5) |
N1—C5 | 1.480 (5) | C4—H4 | 0.9300 |
N1—H1 | 0.9000 | C5—C6 | 1.519 (5) |
N1—H2 | 0.9000 | C5—H5 | 0.9700 |
O1—C1 | 1.261 (5) | C5—H6 | 0.9700 |
O2—C1 | 1.251 (5) | C6—C7 | 1.517 (6) |
O3—H11 | 0.872 (19) | C6—H7 | 0.9700 |
O4—H14 | 0.863 (19) | C6—H8 | 0.9700 |
O5—H12 | 0.909 (19) | C7—C7iii | 1.525 (7) |
O6—H13 | 0.920 (19) | C7—H9 | 0.9700 |
O7—H16 | 0.91 (6) | C7—H10 | 0.9700 |
O7—H15 | 0.78 (6) | | |
| | | |
N1—Cd1—N1i | 167.00 (16) | O1—C1—C2 | 117.3 (3) |
N1—Cd1—O5 | 95.92 (8) | C4—C2—C3 | 118.6 (3) |
N1i—Cd1—O5 | 95.92 (8) | C4—C2—C1 | 120.3 (3) |
N1—Cd1—O4 | 87.55 (8) | C3—C2—C1 | 121.1 (3) |
N1i—Cd1—O4 | 87.55 (8) | C2—C3—C4ii | 120.4 (4) |
O5—Cd1—O4 | 88.0 (2) | C2—C3—H3 | 119.8 |
N1—Cd1—O6 | 92.06 (8) | C4ii—C3—H3 | 119.8 |
N1i—Cd1—O6 | 92.06 (8) | C2—C4—C3ii | 121.0 (3) |
O5—Cd1—O6 | 95.7 (2) | C2—C4—H4 | 119.5 |
O4—Cd1—O6 | 176.4 (2) | C3ii—C4—H4 | 119.5 |
N1—Cd1—O3 | 84.01 (8) | N1—C5—C6 | 114.7 (3) |
N1i—Cd1—O3 | 84.01 (8) | N1—C5—H5 | 108.6 |
O5—Cd1—O3 | 178.58 (18) | C6—C5—H5 | 108.6 |
O4—Cd1—O3 | 90.63 (17) | N1—C5—H6 | 108.6 |
O6—Cd1—O3 | 85.72 (17) | C6—C5—H6 | 108.6 |
C5—N1—Cd1 | 113.6 (2) | H5—C5—H6 | 107.6 |
C5—N1—H1 | 108.8 | C7—C6—C5 | 112.0 (4) |
Cd1—N1—H1 | 108.8 | C7—C6—H7 | 109.2 |
C5—N1—H2 | 108.8 | C5—C6—H7 | 109.2 |
Cd1—N1—H2 | 108.8 | C7—C6—H8 | 109.2 |
H1—N1—H2 | 107.7 | C5—C6—H8 | 109.2 |
Cd1—O3—H11 | 104 (4) | H7—C6—H8 | 107.9 |
Cd1—O4—H14 | 124 (3) | C6—C7—C7iii | 113.3 (5) |
Cd1—O5—H12 | 116 (4) | C6—C7—H9 | 108.9 |
Cd1—O6—H13 | 117 (3) | C7iii—C7—H9 | 108.9 |
H16—O7—H15 | 105 (5) | C6—C7—H10 | 108.9 |
O2—C1—O1 | 124.1 (3) | C7iii—C7—H10 | 108.9 |
O2—C1—C2 | 118.6 (3) | H9—C7—H10 | 107.7 |
| | | |
N1i—Cd1—N1—C5 | −163.8 (6) | O1—C1—C2—C3 | 179.5 (3) |
O5—Cd1—N1—C5 | 40.6 (3) | C4—C2—C3—C4ii | 0.8 (6) |
O4—Cd1—N1—C5 | 128.3 (3) | C1—C2—C3—C4ii | −178.9 (3) |
O6—Cd1—N1—C5 | −55.4 (3) | C3—C2—C4—C3ii | −0.8 (6) |
O3—Cd1—N1—C5 | −140.8 (3) | C1—C2—C4—C3ii | 178.9 (4) |
O2—C1—C2—C4 | −179.2 (4) | Cd1—N1—C5—C6 | 168.6 (3) |
O1—C1—C2—C4 | −0.2 (5) | N1—C5—C6—C7 | −177.1 (3) |
O2—C1—C2—C3 | 0.5 (6) | C5—C6—C7—C7iii | 179.6 (4) |
Symmetry codes: (i) x, −y+3/2, z; (ii) −x, −y+1, −z+1; (iii) −x+2, −y+1, −z+2. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
N1—H1···O7iv | 0.90 | 2.28 | 3.137 (5) | 159 |
N1—H2···O1 | 0.90 | 2.24 | 3.102 (5) | 162 |
O3—H11···O7iv | 0.87 (2) | 1.87 (2) | 2.740 (4) | 173 (5) |
O5—H12···O2v | 0.91 (2) | 2.31 (3) | 3.186 (5) | 161 (5) |
O6—H13···O2vi | 0.92 (2) | 2.15 (2) | 3.069 (5) | 176 (5) |
O7—H16···O1 | 0.91 (6) | 1.88 (7) | 2.773 (5) | 169 (5) |
O7—H15···O2v | 0.78 (6) | 1.94 (6) | 2.713 (5) | 171 (6) |
Symmetry codes: (iv) x, y, z+1; (v) x+1, y, z; (vi) x+1, y, z+1. |