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In the crystal structure of the yellow copper(I) compound, {[Cu2(SO4)(C10H8N2)2]·4H2O}n, one [(C10H8N2)2Cu]n chain is stacked over another [Cu...Cu = 3.180 (1) Å]; the two chains are bridged by SO4 groups through two Cu—O bonds into a double-chain motif. The SO4 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 CuI atom exists in a T-shaped environment.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536804014801/bt6475sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536804014801/bt6475Isup2.hkl
Contains datablock I

CCDC reference: 245151

Key indicators

  • Single-crystal X-ray study
  • T = 298 K
  • Mean [sigma](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

Computing details top

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]·4H2OF(000) = 1240
Mr = 607.57Dx = 1.587 Mg m3
Monoclinic, C2/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2ycCell parameters from 2789 reflections
a = 10.825 (1) Åθ = 2.3–24.7°
b = 17.316 (1) ŵ = 1.81 mm1
c = 14.428 (1) ÅT = 298 K
β = 109.907 (1)°Block, yellow
V = 2542.8 (4) Å30.30 × 0.15 × 0.10 mm
Z = 4
Data collection top
Bruker APEX area-detector
diffractometer
2234 independent reflections
Radiation source: fine-focus sealed tube1449 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.039
φ and ω scansθmax = 25.0°, θmin = 2.4°
Absorption correction: multi-scan
(SADABS; Bruker, 2002)
h = 1212
Tmin = 0.675, Tmax = 0.840k = 2020
11348 measured reflectionsl = 1717
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.066Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.221H-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 parametersΔρmax = 1.27 e Å3
48 restraintsΔρmin = 0.41 e Å3
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Cu10.59148 (8)0.04495 (5)0.18403 (6)0.0691 (5)
S10.50000.2225 (2)0.25000.112 (2)
O10.5777 (6)0.1736 (4)0.2079 (6)0.135 (3)
O20.4114 (6)0.2698 (4)0.1726 (7)0.141 (3)
O1w0.142 (1)0.2934 (9)0.156 (1)0.125 (5)0.50
O2w0.041 (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
N10.7690 (5)0.0297 (3)0.2672 (4)0.057 (1)
N21.4256 (5)0.0257 (3)0.5863 (4)0.061 (2)
C10.8478 (6)0.0901 (4)0.3077 (5)0.072 (2)
C20.9770 (6)0.0811 (4)0.3657 (6)0.071 (2)
C31.0321 (6)0.0086 (3)0.3877 (4)0.050 (2)
C40.9518 (6)0.0528 (3)0.3466 (5)0.061 (2)
C50.8226 (6)0.0414 (3)0.2884 (5)0.061 (2)
C61.3748 (7)0.0452 (4)0.5632 (6)0.069 (2)
C71.2503 (6)0.0580 (4)0.4990 (6)0.071 (2)
C81.1689 (6)0.0027 (3)0.4527 (4)0.051 (2)
C91.2250 (7)0.0745 (4)0.4728 (6)0.081 (3)
C101.3492 (7)0.0847 (4)0.5382 (6)0.083 (3)
H10.81310.13980.29580.087*
H21.02820.12450.39050.085*
H40.98500.10280.35820.073*
H50.77040.08420.26280.074*
H61.42650.08750.59190.083*
H71.21960.10840.48620.085*
H91.17730.11730.44120.097*
H101.38260.13460.55000.099*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Cu10.0440 (6)0.0751 (7)0.0585 (6)0.0026 (4)0.0212 (4)0.0032 (4)
S10.0493 (15)0.0331 (13)0.188 (4)0.0000.0438 (19)0.000
O10.086 (4)0.060 (4)0.188 (7)0.010 (3)0.045 (4)0.029 (4)
O20.066 (4)0.079 (4)0.226 (8)0.010 (3)0.017 (4)0.057 (5)
O1w0.088 (9)0.11 (1)0.17 (1)0.007 (8)0.032 (9)0.02 (1)
O2w0.20 (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)
N10.046 (3)0.059 (3)0.044 (3)0.002 (2)0.013 (2)0.006 (2)
N20.049 (3)0.064 (3)0.049 (3)0.010 (3)0.011 (3)0.004 (3)
C10.056 (4)0.051 (4)0.078 (5)0.015 (3)0.018 (3)0.010 (4)
C20.049 (4)0.051 (4)0.081 (5)0.004 (3)0.020 (3)0.014 (4)
C30.048 (3)0.049 (3)0.037 (3)0.009 (3)0.005 (3)0.007 (3)
C40.053 (4)0.045 (4)0.064 (4)0.006 (3)0.008 (3)0.004 (3)
C50.053 (4)0.052 (4)0.057 (4)0.001 (3)0.010 (3)0.002 (3)
C60.050 (4)0.058 (4)0.071 (5)0.003 (3)0.017 (3)0.003 (3)
C70.057 (4)0.054 (4)0.070 (5)0.005 (3)0.020 (3)0.002 (3)
C80.043 (3)0.053 (4)0.039 (3)0.011 (3)0.009 (3)0.005 (3)
C90.061 (4)0.053 (4)0.086 (5)0.009 (3)0.030 (4)0.020 (4)
C100.069 (5)0.055 (4)0.083 (5)0.023 (4)0.030 (4)0.015 (4)
Geometric parameters (Å, º) top
Cu1—N11.905 (5)C3—C81.471 (8)
Cu1—N2i1.897 (5)C4—C51.378 (7)
Cu1—O12.266 (6)C6—C71.369 (7)
S1—O11.463 (8)C7—C81.388 (7)
S1—O1ii1.463 (8)C8—C91.370 (7)
S1—O21.452 (7)C9—C101.365 (7)
S1—O2ii1.452 (7)C1—H10.93
N1—C11.350 (7)C2—H20.93
N1—C51.351 (6)C4—H40.93
N2—C61.339 (7)C5—H50.93
N2—C101.349 (7)C6—H60.93
C1—C21.373 (7)C7—H70.93
C2—C31.381 (7)C9—H90.93
C3—C41.373 (7)C10—H100.93
N1—Cu1—N2i160.0 (2)N2—C6—C7122.9 (6)
N1—Cu1—O198.3 (2)C6—C7—C8121.4 (6)
N2i—Cu1—O1101.0 (2)C9—C8—C7114.9 (5)
O2ii—S1—O2111.3 (7)C9—C8—C3122.2 (5)
O2ii—S1—O1ii109.2 (5)C7—C8—C3122.9 (5)
O2—S1—O1ii108.9 (4)C10—C9—C8121.7 (6)
O2ii—S1—O1108.9 (4)N2—C10—C9122.9 (6)
O2—S1—O1109.2 (5)N1—C1—H1118.7
O1ii—S1—O1109.2 (7)C2—C1—H1118.7
S1—O1—Cu1135.2 (5)C1—C2—H2119.5
C1—N1—C5116.6 (5)C3—C2—H2119.5
C1—N1—Cu1121.2 (4)C3—C4—H4119.5
C5—N1—Cu1122.2 (4)C5—C4—H4119.5
C6—N2—C10116.0 (6)N1—C5—H5118.7
C6—N2—Cu1iii123.4 (4)C4—C5—H5118.7
C10—N2—Cu1iii120.6 (4)N2—C6—H6118.6
N1—C1—C2122.6 (6)C7—C6—H6118.6
C1—C2—C3120.9 (6)C6—C7—H7119.3
C4—C3—C2116.4 (5)C8—C7—H7119.3
C4—C3—C8121.7 (5)C10—C9—H9119.1
C2—C3—C8122.0 (5)C8—C9—H9119.1
C3—C4—C5120.9 (6)N2—C10—H10118.5
N1—C5—C4122.5 (6)C9—C10—H10118.5
O2ii—S1—O1—Cu1124.9 (6)Cu1—N1—C5—C4178.4 (6)
O2—S1—O1—Cu1113.3 (6)C3—C4—C5—N11 (1)
O1ii—S1—O1—Cu15.6 (3)C10—N2—C6—C74 (1)
N2i—Cu1—O1—S168.1 (6)Cu1iii—N2—C6—C7174.0 (6)
N1—Cu1—O1—S1116.9 (6)N2—C6—C7—C81 (1)
N2i—Cu1—N1—C1157.2 (7)C6—C7—C8—C93 (1)
O1—Cu1—N1—C18.3 (7)C6—C7—C8—C3176.5 (7)
N2i—Cu1—N1—C523 (1)C4—C3—C8—C93 (1)
O1—Cu1—N1—C5171.9 (6)C2—C3—C8—C9178.4 (8)
C5—N1—C1—C22 (1)C4—C3—C8—C7176.8 (7)
Cu1—N1—C1—C2178.2 (7)C2—C3—C8—C72 (1)
N1—C1—C2—C32 (1)C7—C8—C9—C104 (1)
C1—C2—C3—C42 (1)C3—C8—C9—C10175.8 (8)
C1—C2—C3—C8177.6 (7)C6—N2—C10—C93 (1)
C2—C3—C4—C51 (1)Cu1iii—N2—C10—C9174.8 (7)
C8—C3—C4—C5177.9 (7)C8—C9—C10—N21 (1)
C1—N1—C5—C41 (1)
Symmetry codes: (i) x1, y, z1/2; (ii) x+1, y, z+1/2; (iii) x+1, y, z+1/2.
 

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