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In the crystal structure of the yellow copper(I) compound, {[Cu
2(SO
4)(C
10H
8N
2)
2]·4H
2O}
n, one [(C
10H
8N
2)
2Cu]
n chain is stacked over another [Cu
Cu = 3.180 (1) Å]; the two chains are bridged by SO
4 groups through two Cu—O bonds into a double-chain motif. The SO
4 groups are located alternately on opposite sides of the double chain and lie on twofold rotation axes. The disordered solvent water molecules occupy the space between the double chains. The Cu
I atom exists in a T-shaped environment.
Supporting information
CCDC reference: 245151
Key indicators
- Single-crystal X-ray study
- T = 298 K
- Mean (C-C) = 0.010 Å
- H-atom completeness 67%
- Disorder in solvent or counterion
- R factor = 0.066
- wR factor = 0.221
- Data-to-parameter ratio = 12.6
checkCIF/PLATON results
No syntax errors found
Alert level A
PLAT430_ALERT_2_A Short Inter D...A Contact O1W' .. O2W .. 1.99 Ang.
| Author Response: For the two disordered water molecules, O1w and O2w belong to a
pair and O1w' and O2w' another pair.
|
PLAT430_ALERT_2_A Short Inter D...A Contact O2W' .. O2W .. 2.38 Ang.
| Author Response: For the two disordered water molecules, O1w and O2w belong to a
pair and O1w' and O2w' another pair.
|
Alert level B
PLAT241_ALERT_2_B Check High U(eq) as Compared to Neighbors .... O1
PLAT250_ALERT_2_B Large U3/U1 Ratio for Average U(i,j) Tensor .... 4.08
PLAT430_ALERT_2_B Short Inter D...A Contact O1W' .. O2 .. 2.82 Ang.
| Author Response: For the two disordered water molecules, O1w and O2w belong to a
pair and O1w' and O2w' another pair.
|
Alert level C
CHEMW03_ALERT_2_C The ratio of given/expected molecular weight as
calculated from the _atom_site* data lies outside
the range 0.99 <> 1.01
From the CIF: _cell_formula_units_Z 4
From the CIF: _chemical_formula_weight 607.57
TEST: Calculate formula weight from _atom_site_*
atom mass num sum
C 12.01 20.00 240.22
H 1.01 16.00 16.13
N 14.01 4.00 56.03
O 16.00 8.00 127.99
S 32.07 1.00 32.07
Cu 63.55 2.00 127.09
Calculated formula weight 599.53
PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings Differ .... ?
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ?
PLAT043_ALERT_1_C Check Reported Molecular Weight ................ 607.57
PLAT044_ALERT_1_C Calculated and Reported Dx Differ .............. ?
PLAT045_ALERT_1_C Calculated and Reported Z Differ by ............ 0.50 Ratio
PLAT068_ALERT_1_C Reported F000 Differs from Calcd (or Missing)... ?
PLAT094_ALERT_2_C Ratio of Maximum / Minimum Residual Density .... 3.10
PLAT152_ALERT_1_C Supplied and Calc Volume s.u. Inconsistent ..... ?
PLAT242_ALERT_2_C Check Low U(eq) as Compared to Neighbors .... Cu1
PLAT242_ALERT_2_C Check Low U(eq) as Compared to Neighbors .... S1
PLAT242_ALERT_2_C Check Low U(eq) as Compared to Neighbors .... C8
PLAT302_ALERT_4_C Anion/Solvent Disorder ......................... 50.00 Perc.
PLAT341_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 10
PLAT430_ALERT_2_C Short Inter D...A Contact O1 .. O2W .. 2.89 Ang.
| Author Response: For the two disordered water molecules, O1w and O2w belong to a
pair and O1w' and O2w' another pair.
|
PLAT430_ALERT_2_C Short Inter D...A Contact O1W .. O2W .. 2.86 Ang.
| Author Response: For the two disordered water molecules, O1w and O2w belong to a
pair and O1w' and O2w' another pair.
|
PLAT430_ALERT_2_C Short Inter D...A Contact O1W .. O2 .. 2.87 Ang.
| Author Response: For the two disordered water molecules, O1w and O2w belong to a
pair and O1w' and O2w' another pair.
|
PLAT430_ALERT_2_C Short Inter D...A Contact O2 .. O2W .. 2.89 Ang.
| Author Response: For the two disordered water molecules, O1w and O2w belong to a
pair and O1w' and O2w' another pair.
|
PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 2
PLAT733_ALERT_1_C Torsion Calc 5.6(8), Rep 5.6(3) ...... 2.67 su-Rat
O1 -S1 -O1 -CU1 2.655 1.555 1.555 1.555
Alert level G
FORMU01_ALERT_2_G There is a discrepancy between the atom counts in the
_chemical_formula_sum and the formula from the _atom_site* data.
Atom count from _chemical_formula_sum:C20 H24 Cu2 N4 O8 S1
Atom count from the _atom_site data: C20 H16 Cu2 N4 O8 S1
CELLZ01_ALERT_1_G Difference between formula and atom_site contents detected.
CELLZ01_ALERT_1_G WARNING: H atoms missing from atom site list. Is this intentional?
From the CIF: _cell_formula_units_Z 4
From the CIF: _chemical_formula_sum C20 H24 Cu2 N4 O8 S
TEST: Compare cell contents of formula and atom_site data
atom Z*formula cif sites diff
C 80.00 80.00 0.00
H 96.00 64.00 32.00
Cu 8.00 8.00 0.00
N 16.00 16.00 0.00
O 32.00 32.00 0.00
S 4.00 4.00 0.00
2 ALERT level A = In general: serious problem
3 ALERT level B = Potentially serious problem
20 ALERT level C = Check and explain
3 ALERT level G = General alerts; check
10 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
15 ALERT type 2 Indicator that the structure model may be wrong or deficient
1 ALERT type 3 Indicator that the structure quality may be low
2 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: SMART (Bruker, 2002); cell refinement: SAINT (Bruker, 2002); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEPII (Johnson, 1976); software used to prepare material for publication: SHELXL97.
catena-Poly[[[µ-sulfato-dicopper(I)]-di-µ-4,4'-bipyridine-
1:1'
κ2N,
N';2:2'
κ2N,
N'] tetrahydrate]
top
Crystal data top
[Cu2(SO4)(C10H8N2)2]·4H2O | F(000) = 1240 |
Mr = 607.57 | Dx = 1.587 Mg m−3 |
Monoclinic, C2/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -C 2yc | Cell parameters from 2789 reflections |
a = 10.825 (1) Å | θ = 2.3–24.7° |
b = 17.316 (1) Å | µ = 1.81 mm−1 |
c = 14.428 (1) Å | T = 298 K |
β = 109.907 (1)° | Block, yellow |
V = 2542.8 (4) Å3 | 0.30 × 0.15 × 0.10 mm |
Z = 4 | |
Data collection top
Bruker APEX area-detector diffractometer | 2234 independent reflections |
Radiation source: fine-focus sealed tube | 1449 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.039 |
φ and ω scans | θmax = 25.0°, θmin = 2.4° |
Absorption correction: multi-scan (SADABS; Bruker, 2002) | h = −12→12 |
Tmin = 0.675, Tmax = 0.840 | k = −20→20 |
11348 measured reflections | l = −17→17 |
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)] = 0.066 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.221 | H-atom parameters constrained |
S = 1.11 | w = 1/[σ2(Fo2) + (0.1121P)2 + 9.1371P] where P = (Fo2 + 2Fc2)/3 |
2234 reflections | (Δ/σ)max = 0.001 |
177 parameters | Δρmax = 1.27 e Å−3 |
48 restraints | Δρmin = −0.41 e Å−3 |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | Occ. (<1) |
Cu1 | 0.59148 (8) | 0.04495 (5) | 0.18403 (6) | 0.0691 (5) | |
S1 | 0.5000 | 0.2225 (2) | 0.2500 | 0.112 (2) | |
O1 | 0.5777 (6) | 0.1736 (4) | 0.2079 (6) | 0.135 (3) | |
O2 | 0.4114 (6) | 0.2698 (4) | 0.1726 (7) | 0.141 (3) | |
O1w | 0.142 (1) | 0.2934 (9) | 0.156 (1) | 0.125 (5) | 0.50 |
O2w | −0.041 (2) | 0.242 (1) | −0.028 (2) | 0.165 (7) | 0.50 |
O1w' | 0.143 (2) | 0.2463 (9) | 0.066 (1) | 0.146 (7) | 0.50 |
O2w' | −0.272 (2) | 0.2515 (9) | −0.108 (2) | 0.148 (6) | 0.50 |
N1 | 0.7690 (5) | 0.0297 (3) | 0.2672 (4) | 0.057 (1) | |
N2 | 1.4256 (5) | −0.0257 (3) | 0.5863 (4) | 0.061 (2) | |
C1 | 0.8478 (6) | 0.0901 (4) | 0.3077 (5) | 0.072 (2) | |
C2 | 0.9770 (6) | 0.0811 (4) | 0.3657 (6) | 0.071 (2) | |
C3 | 1.0321 (6) | 0.0086 (3) | 0.3877 (4) | 0.050 (2) | |
C4 | 0.9518 (6) | −0.0528 (3) | 0.3466 (5) | 0.061 (2) | |
C5 | 0.8226 (6) | −0.0414 (3) | 0.2884 (5) | 0.061 (2) | |
C6 | 1.3748 (7) | 0.0452 (4) | 0.5632 (6) | 0.069 (2) | |
C7 | 1.2503 (6) | 0.0580 (4) | 0.4990 (6) | 0.071 (2) | |
C8 | 1.1689 (6) | −0.0027 (3) | 0.4527 (4) | 0.051 (2) | |
C9 | 1.2250 (7) | −0.0745 (4) | 0.4728 (6) | 0.081 (3) | |
C10 | 1.3492 (7) | −0.0847 (4) | 0.5382 (6) | 0.083 (3) | |
H1 | 0.8131 | 0.1398 | 0.2958 | 0.087* | |
H2 | 1.0282 | 0.1245 | 0.3905 | 0.085* | |
H4 | 0.9850 | −0.1028 | 0.3582 | 0.073* | |
H5 | 0.7704 | −0.0842 | 0.2628 | 0.074* | |
H6 | 1.4265 | 0.0875 | 0.5919 | 0.083* | |
H7 | 1.2196 | 0.1084 | 0.4862 | 0.085* | |
H9 | 1.1773 | −0.1173 | 0.4412 | 0.097* | |
H10 | 1.3826 | −0.1346 | 0.5500 | 0.099* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Cu1 | 0.0440 (6) | 0.0751 (7) | 0.0585 (6) | −0.0026 (4) | −0.0212 (4) | 0.0032 (4) |
S1 | 0.0493 (15) | 0.0331 (13) | 0.188 (4) | 0.000 | −0.0438 (19) | 0.000 |
O1 | 0.086 (4) | 0.060 (4) | 0.188 (7) | 0.010 (3) | −0.045 (4) | −0.029 (4) |
O2 | 0.066 (4) | 0.079 (4) | 0.226 (8) | 0.010 (3) | −0.017 (4) | 0.057 (5) |
O1w | 0.088 (9) | 0.11 (1) | 0.17 (1) | −0.007 (8) | 0.032 (9) | 0.02 (1) |
O2w | 0.20 (2) | 0.12 (1) | 0.16 (1) | −0.059 (11) | 0.05 (1) | 0.00 (1) |
O1w' | 0.14 (1) | 0.11 (1) | 0.17 (1) | −0.003 (9) | 0.02 (1) | 0.05 (1) |
O2w' | 0.17 (1) | 0.10 (1) | 0.16 (1) | 0.02 (1) | 0.03 (1) | −0.003 (9) |
N1 | 0.046 (3) | 0.059 (3) | 0.044 (3) | 0.002 (2) | −0.013 (2) | −0.006 (2) |
N2 | 0.049 (3) | 0.064 (3) | 0.049 (3) | 0.010 (3) | −0.011 (3) | −0.004 (3) |
C1 | 0.056 (4) | 0.051 (4) | 0.078 (5) | 0.015 (3) | −0.018 (3) | −0.010 (4) |
C2 | 0.049 (4) | 0.051 (4) | 0.081 (5) | 0.004 (3) | −0.020 (3) | −0.014 (4) |
C3 | 0.048 (3) | 0.049 (3) | 0.037 (3) | 0.009 (3) | −0.005 (3) | −0.007 (3) |
C4 | 0.053 (4) | 0.045 (4) | 0.064 (4) | 0.006 (3) | −0.008 (3) | −0.004 (3) |
C5 | 0.053 (4) | 0.052 (4) | 0.057 (4) | 0.001 (3) | −0.010 (3) | −0.002 (3) |
C6 | 0.050 (4) | 0.058 (4) | 0.071 (5) | −0.003 (3) | −0.017 (3) | −0.003 (3) |
C7 | 0.057 (4) | 0.054 (4) | 0.070 (5) | 0.005 (3) | −0.020 (3) | −0.002 (3) |
C8 | 0.043 (3) | 0.053 (4) | 0.039 (3) | 0.011 (3) | −0.009 (3) | −0.005 (3) |
C9 | 0.061 (4) | 0.053 (4) | 0.086 (5) | 0.009 (3) | −0.030 (4) | −0.020 (4) |
C10 | 0.069 (5) | 0.055 (4) | 0.083 (5) | 0.023 (4) | −0.030 (4) | −0.015 (4) |
Geometric parameters (Å, º) top
Cu1—N1 | 1.905 (5) | C3—C8 | 1.471 (8) |
Cu1—N2i | 1.897 (5) | C4—C5 | 1.378 (7) |
Cu1—O1 | 2.266 (6) | C6—C7 | 1.369 (7) |
S1—O1 | 1.463 (8) | C7—C8 | 1.388 (7) |
S1—O1ii | 1.463 (8) | C8—C9 | 1.370 (7) |
S1—O2 | 1.452 (7) | C9—C10 | 1.365 (7) |
S1—O2ii | 1.452 (7) | C1—H1 | 0.93 |
N1—C1 | 1.350 (7) | C2—H2 | 0.93 |
N1—C5 | 1.351 (6) | C4—H4 | 0.93 |
N2—C6 | 1.339 (7) | C5—H5 | 0.93 |
N2—C10 | 1.349 (7) | C6—H6 | 0.93 |
C1—C2 | 1.373 (7) | C7—H7 | 0.93 |
C2—C3 | 1.381 (7) | C9—H9 | 0.93 |
C3—C4 | 1.373 (7) | C10—H10 | 0.93 |
| | | |
N1—Cu1—N2i | 160.0 (2) | N2—C6—C7 | 122.9 (6) |
N1—Cu1—O1 | 98.3 (2) | C6—C7—C8 | 121.4 (6) |
N2i—Cu1—O1 | 101.0 (2) | C9—C8—C7 | 114.9 (5) |
O2ii—S1—O2 | 111.3 (7) | C9—C8—C3 | 122.2 (5) |
O2ii—S1—O1ii | 109.2 (5) | C7—C8—C3 | 122.9 (5) |
O2—S1—O1ii | 108.9 (4) | C10—C9—C8 | 121.7 (6) |
O2ii—S1—O1 | 108.9 (4) | N2—C10—C9 | 122.9 (6) |
O2—S1—O1 | 109.2 (5) | N1—C1—H1 | 118.7 |
O1ii—S1—O1 | 109.2 (7) | C2—C1—H1 | 118.7 |
S1—O1—Cu1 | 135.2 (5) | C1—C2—H2 | 119.5 |
C1—N1—C5 | 116.6 (5) | C3—C2—H2 | 119.5 |
C1—N1—Cu1 | 121.2 (4) | C3—C4—H4 | 119.5 |
C5—N1—Cu1 | 122.2 (4) | C5—C4—H4 | 119.5 |
C6—N2—C10 | 116.0 (6) | N1—C5—H5 | 118.7 |
C6—N2—Cu1iii | 123.4 (4) | C4—C5—H5 | 118.7 |
C10—N2—Cu1iii | 120.6 (4) | N2—C6—H6 | 118.6 |
N1—C1—C2 | 122.6 (6) | C7—C6—H6 | 118.6 |
C1—C2—C3 | 120.9 (6) | C6—C7—H7 | 119.3 |
C4—C3—C2 | 116.4 (5) | C8—C7—H7 | 119.3 |
C4—C3—C8 | 121.7 (5) | C10—C9—H9 | 119.1 |
C2—C3—C8 | 122.0 (5) | C8—C9—H9 | 119.1 |
C3—C4—C5 | 120.9 (6) | N2—C10—H10 | 118.5 |
N1—C5—C4 | 122.5 (6) | C9—C10—H10 | 118.5 |
| | | |
O2ii—S1—O1—Cu1 | 124.9 (6) | Cu1—N1—C5—C4 | 178.4 (6) |
O2—S1—O1—Cu1 | −113.3 (6) | C3—C4—C5—N1 | 1 (1) |
O1ii—S1—O1—Cu1 | 5.6 (3) | C10—N2—C6—C7 | 4 (1) |
N2i—Cu1—O1—S1 | 68.1 (6) | Cu1iii—N2—C6—C7 | −174.0 (6) |
N1—Cu1—O1—S1 | −116.9 (6) | N2—C6—C7—C8 | −1 (1) |
N2i—Cu1—N1—C1 | 157.2 (7) | C6—C7—C8—C9 | −3 (1) |
O1—Cu1—N1—C1 | −8.3 (7) | C6—C7—C8—C3 | 176.5 (7) |
N2i—Cu1—N1—C5 | −23 (1) | C4—C3—C8—C9 | 3 (1) |
O1—Cu1—N1—C5 | 171.9 (6) | C2—C3—C8—C9 | −178.4 (8) |
C5—N1—C1—C2 | 2 (1) | C4—C3—C8—C7 | −176.8 (7) |
Cu1—N1—C1—C2 | −178.2 (7) | C2—C3—C8—C7 | 2 (1) |
N1—C1—C2—C3 | −2 (1) | C7—C8—C9—C10 | 4 (1) |
C1—C2—C3—C4 | 2 (1) | C3—C8—C9—C10 | −175.8 (8) |
C1—C2—C3—C8 | −177.6 (7) | C6—N2—C10—C9 | −3 (1) |
C2—C3—C4—C5 | −1 (1) | Cu1iii—N2—C10—C9 | 174.8 (7) |
C8—C3—C4—C5 | 177.9 (7) | C8—C9—C10—N2 | −1 (1) |
C1—N1—C5—C4 | −1 (1) | | |
Symmetry codes: (i) x−1, −y, z−1/2; (ii) −x+1, y, −z+1/2; (iii) x+1, −y, z+1/2. |
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