The title compound, {[Cu2(C10H8N2)3](ClO4)2·2H2O}n, forms a three-dimensional network containing one-dimensional nanoporous channels, accommodating guest water molecules and perchlorate anions. The network consists of [Cu2(4,4′-bipyridyl)3]2+ cations containing trigonal planar CuI centers bonded to three 4,4′-bipyridyl groups.
Supporting information
CCDC reference: 238684
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (C-C) = 0.007 Å
- Disorder in solvent or counterion
- R factor = 0.053
- wR factor = 0.169
- Data-to-parameter ratio = 12.2
checkCIF/PLATON results
No syntax errors found
Alert level C
PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings Differ .... ?
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ?
PLAT045_ALERT_1_C Calculated and Reported Z Differ by ............ 2.00 Ratio
PLAT062_ALERT_4_C Rescale T(min) & T(max) by ..................... 0.72
PLAT244_ALERT_4_C Low Solvent U(eq) as Compared to Neighbors .... Cl1
PLAT302_ALERT_4_C Anion/Solvent Disorder ......................... 8.00 Perc.
PLAT341_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 7
PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 2
Alert level G
ABSTM02_ALERT_3_G When printed, the submitted absorption T values will be
replaced by the scaled T values. Since the ratio of scaled T's
is identical to the ratio of reported T values, the scaling
does not imply a change to the absorption corrections used in
the study.
Ratio of Tmax expected/reported 0.719
Tmax scaled 0.719 Tmin scaled 0.538
0 ALERT level A = In general: serious problem
0 ALERT level B = Potentially serious problem
8 ALERT level C = Check and explain
1 ALERT level G = General alerts; check
3 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
0 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
4 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: SMART (Siemens, 1996); cell refinement: SMART and SAINT (Siemens,1994); data reduction: SAINT and XPREP in SHELXTL (Siemens, 1994); program(s) used to solve structure: SHELXTL; program(s) used to refine structure: SHELXTL; molecular graphics: SHELXTL; software used to prepare material for publication: SHELXTL.
Poly[[dicopper(I)-tri-µ-4,4'-bipyridyl] diperchlorate dihydrate]
top
Crystal data top
[Cu2(C10H8N2)3](ClO4)2·2H2O | F(000) = 6752 |
Mr = 830.56 | Dx = 1.654 Mg m−3 |
Orthorhombic, Fddd | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -F 2uv 2vw | Cell parameters from 200 reflections |
a = 18.7770 (8) Å | θ = 1.5–25.0° |
b = 23.3593 (13) Å | µ = 1.50 mm−1 |
c = 30.4231 (16) Å | T = 293 K |
V = 13344.1 (12) Å3 | Prism, yellow |
Z = 16 | 0.56 × 0.40 × 0.22 mm |
Data collection top
SMART CCD area-detector diffractometer | 2938 independent reflections |
Radiation source: fine-focus sealed tube | 2014 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.038 |
φ and ω scans | θmax = 25.0°, θmin = 1.5° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −22→12 |
Tmin = 0.538, Tmax = 0.719 | k = −19→27 |
7804 measured reflections | l = −35→35 |
Refinement top
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.053 | H atoms treated by a mixture of independent and constrained refinement |
wR(F2) = 0.169 | w = 1/[σ2(Fo2) + (0.089P)2 + 84.2861P] where P = (Fo2 + 2Fc2)/3 |
S = 1.00 | (Δ/σ)max = 0.004 |
2938 reflections | Δρmax = 0.62 e Å−3 |
241 parameters | Δρmin = −0.36 e Å−3 |
0 restraints | Extinction correction: SHELXTL, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
Primary atom site location: structure-invariant direct methods | Extinction coefficient: 0.00015 (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 | Occ. (<1) |
Cu1 | 0.23583 (4) | 0.36023 (3) | 0.12145 (2) | 0.0559 (3) | |
N1 | 0.2878 (2) | 0.40542 (18) | 0.16730 (14) | 0.0478 (10) | |
N2 | 0.4371 (2) | 0.58827 (17) | 0.32842 (14) | 0.0490 (10) | |
N3 | 0.2292 (2) | 0.27642 (18) | 0.12170 (13) | 0.0497 (11) | |
C1 | 0.3266 (3) | 0.4513 (2) | 0.15647 (17) | 0.0531 (13) | |
H1 | 0.3336 | 0.4590 | 0.1268 | 0.064* | |
C2 | 0.3564 (3) | 0.4875 (2) | 0.18631 (18) | 0.0517 (13) | |
H2 | 0.3822 | 0.5191 | 0.1767 | 0.062* | |
C3 | 0.2809 (3) | 0.3951 (2) | 0.21022 (18) | 0.0518 (13) | |
H3 | 0.2555 | 0.3628 | 0.2187 | 0.062* | |
C4 | 0.3090 (3) | 0.4291 (2) | 0.24246 (17) | 0.0489 (13) | |
H4 | 0.3019 | 0.4200 | 0.2719 | 0.059* | |
C5 | 0.3484 (3) | 0.4774 (2) | 0.23094 (16) | 0.0431 (11) | |
C6 | 0.3795 (2) | 0.5151 (2) | 0.26475 (17) | 0.0434 (11) | |
C7 | 0.4042 (3) | 0.4946 (2) | 0.30455 (17) | 0.0534 (13) | |
H7 | 0.4020 | 0.4557 | 0.3107 | 0.064* | |
C8 | 0.4321 (3) | 0.5315 (2) | 0.33479 (17) | 0.0546 (13) | |
H8 | 0.4484 | 0.5166 | 0.3613 | 0.066* | |
C9 | 0.3856 (3) | 0.5741 (2) | 0.25745 (18) | 0.0500 (13) | |
H9 | 0.3709 | 0.5898 | 0.2309 | 0.060* | |
C10 | 0.4136 (3) | 0.6085 (2) | 0.28969 (18) | 0.0522 (13) | |
H10 | 0.4164 | 0.6477 | 0.2845 | 0.063* | |
C11 | 0.2499 (3) | 0.2454 (2) | 0.08708 (18) | 0.0580 (14) | |
H11 | 0.2644 | 0.2644 | 0.0618 | 0.070* | |
C12 | 0.2506 (3) | 0.1863 (2) | 0.08723 (18) | 0.0562 (14) | |
H12 | 0.2651 | 0.1664 | 0.0623 | 0.067* | |
C13 | 0.2077 (3) | 0.2476 (2) | 0.15745 (18) | 0.0549 (13) | |
H13 | 0.1918 | 0.2684 | 0.1816 | 0.066* | |
C14 | 0.2079 (3) | 0.1889 (2) | 0.15999 (17) | 0.0522 (13) | |
H14 | 0.1935 | 0.1709 | 0.1857 | 0.063* | |
C15 | 0.2296 (3) | 0.1568 (2) | 0.12447 (16) | 0.0444 (12) | |
Cl1 | 0.3750 | 0.3750 | 0.02855 (6) | 0.0610 (5) | |
O1 | 0.3227 (7) | 0.4218 (5) | 0.0195 (4) | 0.123 (4) | 0.50 |
O2 | 0.3258 (6) | 0.3438 (5) | 0.0079 (3) | 0.203 (5) | |
O3 | 0.3750 | 0.3750 | 0.0733 (2) | 0.151 (4) | |
Cl2 | 0.77566 (13) | 0.1250 | 0.1250 | 0.0644 (6) | |
O4 | 0.7344 (5) | 0.1631 (4) | 0.1024 (3) | 0.183 (4) | |
O5 | 0.8155 (6) | 0.0955 (5) | 0.0973 (3) | 0.239 (5) | |
O1W | 0.3346 (5) | 0.5398 (4) | 0.0138 (3) | 0.124 (3) | |
H1WA | 0.338 (5) | 0.549 (4) | 0.037 (3) | 0.10 (3)* | |
H1WB | 0.325 (5) | 0.506 (4) | 0.016 (3) | 0.11 (3)* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Cu1 | 0.0744 (5) | 0.0384 (4) | 0.0550 (5) | 0.0011 (3) | −0.0118 (3) | −0.0004 (3) |
N1 | 0.056 (3) | 0.042 (2) | 0.046 (3) | 0.004 (2) | −0.006 (2) | −0.0053 (19) |
N2 | 0.055 (3) | 0.039 (2) | 0.053 (3) | −0.0049 (19) | −0.006 (2) | 0.0002 (19) |
N3 | 0.061 (3) | 0.039 (2) | 0.049 (3) | 0.000 (2) | −0.013 (2) | 0.0001 (19) |
C1 | 0.061 (3) | 0.050 (3) | 0.049 (3) | −0.002 (3) | −0.001 (3) | −0.002 (2) |
C2 | 0.052 (3) | 0.045 (3) | 0.058 (3) | −0.007 (2) | 0.000 (3) | −0.001 (3) |
C3 | 0.054 (3) | 0.042 (3) | 0.060 (4) | 0.002 (2) | −0.004 (3) | −0.002 (2) |
C4 | 0.056 (3) | 0.046 (3) | 0.045 (3) | 0.001 (2) | −0.003 (2) | −0.002 (2) |
C5 | 0.044 (3) | 0.040 (3) | 0.045 (3) | 0.006 (2) | −0.002 (2) | −0.004 (2) |
C6 | 0.038 (3) | 0.043 (3) | 0.050 (3) | −0.001 (2) | −0.001 (2) | −0.005 (2) |
C7 | 0.067 (3) | 0.039 (3) | 0.055 (3) | −0.004 (3) | −0.007 (3) | 0.000 (2) |
C8 | 0.069 (4) | 0.046 (3) | 0.049 (3) | −0.010 (3) | −0.010 (3) | 0.001 (2) |
C9 | 0.053 (3) | 0.044 (3) | 0.053 (3) | 0.002 (2) | −0.009 (2) | 0.001 (2) |
C10 | 0.061 (3) | 0.037 (3) | 0.058 (3) | −0.002 (2) | −0.008 (3) | 0.001 (2) |
C11 | 0.083 (4) | 0.046 (3) | 0.045 (3) | 0.005 (3) | 0.003 (3) | 0.003 (2) |
C12 | 0.077 (4) | 0.044 (3) | 0.047 (3) | 0.004 (3) | 0.005 (3) | −0.006 (2) |
C13 | 0.074 (4) | 0.041 (3) | 0.050 (3) | −0.001 (3) | −0.001 (3) | −0.008 (2) |
C14 | 0.068 (3) | 0.044 (3) | 0.045 (3) | −0.004 (3) | 0.001 (3) | 0.001 (2) |
C15 | 0.050 (3) | 0.036 (3) | 0.046 (3) | −0.003 (2) | −0.002 (2) | 0.002 (2) |
Cl1 | 0.0707 (13) | 0.0704 (12) | 0.0420 (11) | −0.0053 (11) | 0.000 | 0.000 |
O1 | 0.119 (9) | 0.103 (9) | 0.147 (10) | 0.039 (7) | −0.001 (8) | 0.045 (8) |
O2 | 0.237 (10) | 0.251 (11) | 0.122 (6) | −0.147 (9) | −0.029 (6) | −0.006 (6) |
O3 | 0.182 (9) | 0.223 (12) | 0.050 (4) | 0.058 (8) | 0.000 | 0.000 |
Cl2 | 0.0903 (16) | 0.0514 (11) | 0.0516 (11) | 0.000 | 0.000 | 0.0024 (9) |
O4 | 0.221 (9) | 0.144 (7) | 0.183 (8) | 0.045 (6) | −0.054 (7) | 0.059 (6) |
O5 | 0.252 (12) | 0.243 (11) | 0.222 (10) | 0.039 (9) | 0.111 (9) | −0.092 (8) |
O1W | 0.192 (8) | 0.097 (5) | 0.083 (5) | −0.026 (5) | 0.003 (5) | 0.019 (4) |
Geometric parameters (Å, º) top
Cu1—N3 | 1.962 (4) | C1—H1 | 0.93 |
Cu1—N2i | 1.999 (4) | C9—C10 | 1.373 (7) |
Cu1—N1 | 2.003 (4) | C9—H9 | 0.93 |
N3—C11 | 1.336 (6) | C7—C8 | 1.365 (7) |
N3—C13 | 1.342 (6) | C7—H7 | 0.93 |
C6—C7 | 1.382 (7) | C12—H12 | 0.93 |
C6—C9 | 1.401 (7) | C2—H2 | 0.93 |
C6—C5 | 1.474 (7) | Cl1—O2 | 1.335 (7) |
C15—C14 | 1.378 (7) | Cl1—O2iii | 1.335 (7) |
C15—C12 | 1.383 (7) | Cl1—O3 | 1.361 (8) |
C15—C15ii | 1.484 (9) | Cl1—O1iii | 1.496 (10) |
N1—C3 | 1.334 (7) | Cl1—O1 | 1.496 (10) |
N1—C1 | 1.338 (7) | Cl2—O5ii | 1.320 (7) |
C4—C3 | 1.368 (7) | Cl2—O5 | 1.320 (7) |
C4—C5 | 1.394 (7) | Cl2—O4ii | 1.366 (7) |
C4—H4 | 0.93 | Cl2—O4 | 1.366 (7) |
C5—C2 | 1.386 (7) | O1W—H1WB | 0.81 (8) |
C13—C14 | 1.373 (7) | O1W—H1WA | 0.74 (8) |
C13—H13 | 0.93 | N2—C8 | 1.343 (6) |
C11—C12 | 1.381 (7) | N2—C10 | 1.344 (6) |
C11—H11 | 0.93 | N2—Cu1iv | 1.999 (4) |
C14—H14 | 0.93 | C10—H10 | 0.93 |
C3—H3 | 0.93 | C8—H8 | 0.93 |
C1—C2 | 1.361 (7) | | |
| | | |
N3—Cu1—N2i | 125.03 (17) | C10—C9—H9 | 120.2 |
N3—Cu1—N1 | 123.65 (17) | C6—C9—H9 | 120.2 |
N2i—Cu1—N1 | 111.21 (17) | C8—C7—C6 | 120.1 (5) |
C11—N3—C13 | 117.0 (4) | C8—C7—H7 | 120.0 |
C11—N3—Cu1 | 121.3 (4) | C6—C7—H7 | 120.0 |
C13—N3—Cu1 | 121.5 (3) | C11—C12—C15 | 119.9 (5) |
C7—C6—C9 | 116.8 (5) | C11—C12—H12 | 120.1 |
C7—C6—C5 | 122.6 (4) | C15—C12—H12 | 120.1 |
C9—C6—C5 | 120.7 (5) | C1—C2—C5 | 120.2 (5) |
C14—C15—C12 | 117.0 (4) | C1—C2—H2 | 119.9 |
C14—C15—C15ii | 121.9 (5) | C5—C2—H2 | 119.9 |
C12—C15—C15ii | 121.1 (5) | O2—Cl1—O2iii | 123.7 (7) |
C3—N1—C1 | 116.0 (4) | O2—Cl1—O3 | 118.1 (4) |
C3—N1—Cu1 | 122.6 (4) | O2iii—Cl1—O3 | 118.1 (4) |
C1—N1—Cu1 | 121.1 (4) | O2—Cl1—O1iii | 88.2 (7) |
C3—C4—C5 | 119.6 (5) | O2iii—Cl1—O1iii | 81.8 (7) |
C3—C4—H4 | 120.2 | O3—Cl1—O1iii | 100.6 (5) |
C5—C4—H4 | 120.2 | O2—Cl1—O1 | 81.8 (7) |
C2—C5—C4 | 116.2 (5) | O2iii—Cl1—O1 | 88.2 (7) |
C2—C5—C6 | 122.6 (5) | O3—Cl1—O1 | 100.6 (5) |
C4—C5—C6 | 121.2 (5) | O1iii—Cl1—O1 | 158.7 (10) |
N3—C13—C14 | 123.0 (5) | O5ii—Cl2—O5 | 111.0 (11) |
N3—C13—H13 | 118.5 | O5ii—Cl2—O4ii | 109.8 (7) |
C14—C13—H13 | 118.5 | O5—Cl2—O4ii | 107.7 (7) |
N3—C11—C12 | 122.9 (5) | O5ii—Cl2—O4 | 107.7 (7) |
N3—C11—H11 | 118.6 | O5—Cl2—O4 | 109.8 (7) |
C12—C11—H11 | 118.6 | O4ii—Cl2—O4 | 110.9 (8) |
C13—C14—C15 | 120.1 (5) | H1WB—O1W—H1WA | 104 (9) |
C13—C14—H14 | 119.9 | C8—N2—C10 | 116.8 (4) |
C15—C14—H14 | 119.9 | C8—N2—Cu1iv | 122.1 (3) |
N1—C3—C4 | 124.0 (5) | C10—N2—Cu1iv | 120.8 (3) |
N1—C3—H3 | 118.0 | N2—C10—C9 | 123.1 (5) |
C4—C3—H3 | 118.0 | N2—C10—H10 | 118.5 |
N1—C1—C2 | 123.9 (5) | C9—C10—H10 | 118.5 |
N1—C1—H1 | 118.1 | N2—C8—C7 | 123.6 (5) |
C2—C1—H1 | 118.1 | N2—C8—H8 | 118.2 |
C10—C9—C6 | 119.7 (5) | C7—C8—H8 | 118.2 |
Symmetry codes: (i) x−1/4, −y+1, z−1/4; (ii) x, −y+1/4, −z+1/4; (iii) −x+3/4, −y+3/4, z; (iv) x+1/4, −y+1, z+1/4. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O1W—H1WB···O1 | 0.81 (8) | 1.97 (9) | 2.771 (14) | 168 (9) |
O1W—H1WA···O5v | 0.74 (8) | 2.17 (8) | 2.877 (13) | 159 (9) |
Symmetry code: (v) x−1/2, y+1/2, z. |