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The title complex, [Cu2(C7H4O5S)2(C10H9N3)2]·3H2O, comprises the centrosymmetric cyclic dimeric CuII complex and uncoordinated water mol­ecules. The CuII atom displays a distorted square-pyramidal geometry. Within the cyclic dimer, the Cu...Cu separation is 9.5362 (12) Å.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536805020489/xu6023sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536805020489/xu6023Isup2.hkl
Contains datablock I

CCDC reference: 282705

Key indicators

  • Single-crystal X-ray study
  • T = 295 K
  • Mean [sigma](C-C) = 0.008 Å
  • Disorder in main residue
  • R factor = 0.065
  • wR factor = 0.157
  • Data-to-parameter ratio = 11.3

checkCIF/PLATON results

No syntax errors found



Alert level B PLAT241_ALERT_2_B Check High Ueq as Compared to Neighbors for O4' PLAT420_ALERT_2_B D-H Without Acceptor >O1W - >H1A ... ? PLAT420_ALERT_2_B D-H Without Acceptor >O1W - >H1B ... ?
Alert level C PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT220_ALERT_2_C Large Non-Solvent O Ueq(max)/Ueq(min) ... 2.58 Ratio PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for O4 PLAT250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor .... 2.19 PLAT301_ALERT_3_C Main Residue Disorder ......................... 4.00 Perc. PLAT302_ALERT_4_C Anion/Solvent Disorder ......................... 50.00 Perc. PLAT341_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 8 PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 1 PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 2 H2 O
0 ALERT level A = In general: serious problem 3 ALERT level B = Potentially serious problem 9 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 1 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 2 ALERT type 3 Indicator that the structure quality may be low 3 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: ORTEP-3 for Windows (Farrugia, 1997); software used to prepare material for publication: WinGX (Farrugia, 1999).

bis(µ2-4-sulfonatobenzoato)bis[(di-2-pyridylamine)copper(II)] trihydrate top
Crystal data top
[Cu2(C7H4O5S)2(C10H9N3)2]·3H2OZ = 1
Mr = 923.86F(000) = 472
Triclinic, P1Dx = 1.670 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 8.2409 (5) ÅCell parameters from 3422 reflections
b = 9.8064 (6) Åθ = 2.5–27.7°
c = 11.5670 (7) ŵ = 1.35 mm1
α = 87.027 (1)°T = 295 K
β = 85.507 (1)°Block, green
γ = 80.552 (1)°0.38 × 0.19 × 0.16 mm
V = 918.5 (1) Å3
Data collection top
Bruker APEX area-detector
diffractometer
3218 independent reflections
Radiation source: fine-focus sealed tube2979 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.019
φ and ω scansθmax = 25.0°, θmin = 1.8°
Absorption correction: multi-scan
(SADABS; Sheldrick, 2002)
h = 99
Tmin = 0.629, Tmax = 0.813k = 1111
6651 measured reflectionsl = 1313
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)] = 0.065Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.157H-atom parameters constrained
S = 1.17 w = 1/[σ2(Fo2) + (0.0638P)2 + 2.1586P]
where P = (Fo2 + 2Fc2)/3
3218 reflections(Δ/σ)max < 0.001
284 parametersΔρmax = 0.98 e Å3
27 restraintsΔρmin = 0.52 e Å3
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
xyzUiso*/UeqOcc. (<1)
Cu10.57003 (8)0.06038 (6)0.32867 (5)0.0438 (2)
S10.1942 (2)0.70064 (17)0.77512 (17)0.0677 (5)
N10.4495 (5)0.0155 (4)0.2148 (3)0.0389 (9)
N20.6791 (6)0.1749 (4)0.1464 (4)0.0483 (11)
H2N0.71740.22280.08720.058*
N30.7609 (5)0.0860 (4)0.3138 (4)0.0403 (10)
O10.3898 (5)0.2076 (4)0.3839 (3)0.0561 (10)
O20.6015 (5)0.1460 (4)0.4856 (3)0.0480 (9)
O30.0621 (7)0.7827 (6)0.7111 (6)0.124 (3)
O40.1121 (14)0.6450 (13)0.8723 (10)0.068 (3)0.50
O4'0.1908 (19)0.6359 (15)0.8912 (9)0.101 (5)0.50
O50.3221 (6)0.7819 (4)0.7847 (4)0.0687 (13)
O1W0.7930 (14)0.3733 (11)0.0213 (10)0.084 (3)0.57
H1A0.87700.34600.04580.100*0.57
H1B0.75800.40300.07880.100*0.57
O1W'0.713 (2)0.4178 (15)0.0147 (13)0.087 (4)0.43
H1C0.78460.47770.04680.104*0.43
H1D0.73360.40370.05920.104*0.43
O2W0.2059 (13)0.4015 (10)0.2218 (8)0.076 (3)0.50
H1W0.27450.33970.25390.091*0.50
H2W0.11470.37100.22370.091*0.50
C10.2884 (7)0.0387 (6)0.2070 (5)0.0505 (13)
H10.24050.10620.25830.061*
C20.1935 (8)0.0003 (6)0.1282 (5)0.0581 (15)
H20.08340.03980.12540.070*
C30.2641 (8)0.1014 (7)0.0520 (5)0.0594 (15)
H30.20190.13040.00300.071*
C40.4253 (8)0.1576 (6)0.0585 (5)0.0538 (14)
H40.47450.22510.00760.065*
C50.5168 (7)0.1136 (5)0.1419 (4)0.0409 (11)
C60.7901 (6)0.1735 (5)0.2275 (5)0.0432 (12)
C70.9359 (7)0.2695 (6)0.2176 (6)0.0572 (15)
H70.95500.32970.15670.069*
C81.0487 (8)0.2740 (6)0.2972 (7)0.0659 (18)
H81.14540.33800.29190.079*
C91.0193 (8)0.1828 (6)0.3863 (6)0.0647 (17)
H91.09600.18360.44120.078*
C100.8762 (7)0.0919 (5)0.3920 (5)0.0515 (14)
H100.85620.03080.45230.062*
C110.4703 (6)0.2268 (5)0.4691 (4)0.0393 (11)
C120.4057 (6)0.3427 (5)0.5457 (4)0.0346 (10)
C130.2609 (7)0.4286 (5)0.5223 (5)0.0458 (12)
H130.20460.41290.45890.055*
C140.1990 (7)0.5375 (5)0.5920 (5)0.0491 (13)
H140.10170.59520.57520.059*
C150.2805 (6)0.5607 (5)0.6858 (5)0.0444 (12)
C160.4255 (7)0.4766 (6)0.7107 (5)0.0486 (13)
H160.48130.49310.77420.058*
C170.4878 (6)0.3666 (5)0.6397 (4)0.0401 (11)
H170.58550.30910.65600.048*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Cu10.0541 (4)0.0300 (3)0.0461 (4)0.0046 (3)0.0102 (3)0.0163 (3)
S10.0647 (10)0.0518 (9)0.0864 (12)0.0100 (8)0.0226 (9)0.0421 (9)
N10.053 (3)0.028 (2)0.035 (2)0.0024 (18)0.0047 (18)0.0117 (16)
N20.060 (3)0.038 (2)0.042 (2)0.008 (2)0.000 (2)0.0133 (19)
N30.044 (2)0.028 (2)0.049 (2)0.0032 (17)0.0067 (19)0.0048 (18)
O10.065 (2)0.048 (2)0.054 (2)0.0086 (18)0.0165 (19)0.0251 (18)
O20.054 (2)0.0385 (19)0.049 (2)0.0078 (17)0.0081 (17)0.0174 (16)
O30.082 (4)0.102 (4)0.181 (7)0.037 (3)0.021 (4)0.083 (5)
O40.062 (6)0.050 (5)0.088 (6)0.014 (5)0.041 (5)0.022 (5)
O4'0.124 (9)0.065 (7)0.116 (8)0.037 (7)0.050 (7)0.046 (6)
O50.113 (4)0.040 (2)0.056 (3)0.025 (2)0.011 (2)0.0166 (19)
O1W0.080 (7)0.073 (7)0.092 (8)0.003 (5)0.024 (6)0.032 (6)
O1W'0.109 (13)0.076 (10)0.066 (9)0.015 (8)0.001 (8)0.017 (7)
O2W0.084 (6)0.064 (6)0.077 (6)0.000 (5)0.018 (5)0.006 (5)
C10.053 (3)0.046 (3)0.051 (3)0.002 (2)0.004 (3)0.023 (3)
C20.051 (3)0.062 (4)0.061 (4)0.000 (3)0.010 (3)0.021 (3)
C30.065 (4)0.063 (4)0.052 (3)0.007 (3)0.015 (3)0.016 (3)
C40.075 (4)0.041 (3)0.044 (3)0.000 (3)0.004 (3)0.017 (2)
C50.055 (3)0.031 (2)0.035 (3)0.004 (2)0.000 (2)0.006 (2)
C60.049 (3)0.029 (2)0.050 (3)0.002 (2)0.004 (2)0.003 (2)
C70.051 (3)0.039 (3)0.079 (4)0.001 (3)0.004 (3)0.013 (3)
C80.043 (3)0.045 (3)0.108 (5)0.002 (3)0.008 (3)0.009 (3)
C90.062 (4)0.044 (3)0.092 (5)0.007 (3)0.026 (3)0.008 (3)
C100.056 (3)0.029 (3)0.071 (4)0.003 (2)0.015 (3)0.008 (2)
C110.049 (3)0.031 (2)0.038 (3)0.008 (2)0.002 (2)0.008 (2)
C120.039 (3)0.026 (2)0.038 (3)0.0053 (19)0.003 (2)0.0075 (19)
C130.050 (3)0.042 (3)0.047 (3)0.005 (2)0.007 (2)0.012 (2)
C140.046 (3)0.034 (3)0.065 (4)0.000 (2)0.001 (3)0.012 (2)
C150.044 (3)0.032 (3)0.058 (3)0.011 (2)0.015 (2)0.019 (2)
C160.046 (3)0.049 (3)0.054 (3)0.013 (2)0.000 (2)0.023 (3)
C170.037 (3)0.035 (3)0.047 (3)0.001 (2)0.002 (2)0.010 (2)
Geometric parameters (Å, º) top
Cu1—O11.985 (4)C1—H10.9300
Cu1—O22.090 (3)C2—C31.385 (8)
Cu1—O5i2.227 (4)C2—H20.9300
Cu1—N11.956 (4)C3—C41.359 (9)
Cu1—N31.951 (4)C3—H30.9300
Cu1—Cu1i9.5362 (12)C4—C51.396 (7)
S1—O41.399 (8)C4—H40.9300
S1—O51.436 (4)C6—C71.400 (7)
S1—O4'1.456 (9)C7—C81.353 (9)
S1—O31.469 (6)C7—H70.9300
S1—C151.780 (5)C8—C91.381 (9)
N1—C51.334 (6)C8—H80.9300
N1—C11.355 (7)C9—C101.356 (8)
N2—C61.363 (7)C9—H90.9300
N2—C51.377 (7)C10—H100.9300
N2—H2N0.8600C11—C121.480 (6)
N3—C61.332 (7)C12—C171.374 (7)
N3—C101.355 (7)C12—C131.380 (7)
O1—C111.269 (6)C13—C141.377 (7)
O2—C111.252 (6)C13—H130.9300
O1W—H1A0.8090C14—C151.368 (8)
O1W—H1B0.8295C14—H140.9300
O1W'—H1C0.8514C15—C161.378 (8)
O1W'—H1D0.8662C16—C171.395 (7)
O2W—H1W0.8494C16—H160.9300
O2W—H2W0.8516C17—H170.9300
C1—C21.354 (8)
O1—Cu1—O264.16 (14)C2—C3—H3120.4
O1—Cu1—O5i89.24 (17)C3—C4—C5119.8 (5)
O2—Cu1—O5i95.85 (15)C3—C4—H4120.1
N1—Cu1—O197.59 (16)C5—C4—H4120.1
N1—Cu1—O2156.07 (17)N1—C5—N2121.1 (5)
N1—Cu1—O5i99.40 (16)N1—C5—C4121.2 (5)
N3—Cu1—N194.06 (17)N2—C5—C4117.8 (5)
N3—Cu1—O1165.98 (17)N3—C6—N2121.6 (5)
N3—Cu1—O2102.42 (16)N3—C6—C7121.1 (5)
N3—Cu1—O5i96.54 (17)N2—C6—C7117.2 (5)
O4—S1—O5122.4 (6)C8—C7—C6119.5 (6)
O5—S1—O4'99.3 (7)C8—C7—H7120.2
O4—S1—O3104.5 (6)C6—C7—H7120.2
O5—S1—O3109.0 (4)C7—C8—C9119.5 (6)
O4'—S1—O3130.8 (7)C7—C8—H8120.2
O4—S1—C15107.3 (6)C9—C8—H8120.2
O5—S1—C15106.7 (2)C10—C9—C8118.7 (6)
O4'—S1—C15103.2 (6)C10—C9—H9120.7
O3—S1—C15105.9 (3)C8—C9—H9120.7
C5—N1—C1118.0 (4)N3—C10—C9122.9 (6)
C5—N1—Cu1124.3 (4)N3—C10—H10118.5
C1—N1—Cu1117.6 (3)C9—C10—H10118.5
C6—N2—C5131.8 (4)O2—C11—O1118.4 (4)
C6—N2—H2N114.1O2—C11—C12122.5 (5)
C5—N2—H2N114.1O1—C11—C12119.1 (5)
C6—N3—C10118.3 (5)O2—C11—Cu161.8 (2)
C6—N3—Cu1124.2 (4)O1—C11—Cu157.0 (2)
C10—N3—Cu1117.3 (3)C12—C11—Cu1173.4 (4)
C11—O1—Cu190.6 (3)C17—C12—C13119.3 (4)
C11—O2—Cu186.4 (3)C17—C12—C11121.1 (4)
S1—O5—Cu1i135.1 (3)C13—C12—C11119.6 (5)
H1A—O1W—H1B104.6C14—C13—C12120.6 (5)
H1A—O1W—H1C125.5C14—C13—H13119.7
H1B—O1W—H1C98.0C12—C13—H13119.7
H1A—O1W—H1D125.1C15—C14—C13120.0 (5)
H1C—O1W—H1D86.4C15—C14—H14120.0
H1B—O1W'—H1C108.0C13—C14—H14120.0
H1C—O1W'—H1D114.8C14—C15—C16120.5 (5)
H1W—O2W—H2W107.4C14—C15—S1118.6 (4)
C2—C1—N1123.4 (5)C16—C15—S1120.9 (4)
C2—C1—H1118.3C15—C16—C17119.2 (5)
N1—C1—H1118.3C15—C16—H16120.4
C1—C2—C3118.5 (6)C17—C16—H16120.4
C1—C2—H2120.7C12—C17—C16120.4 (5)
C3—C2—H2120.7C12—C17—H17119.8
C4—C3—C2119.1 (5)C16—C17—H17119.8
C4—C3—H3120.4
N3—Cu1—N1—C513.7 (4)C3—C4—C5—N2179.0 (5)
O1—Cu1—N1—C5174.1 (4)C10—N3—C6—N2179.2 (5)
O2—Cu1—N1—C5147.5 (4)Cu1—N3—C6—N25.7 (7)
O5i—Cu1—N1—C583.7 (4)C10—N3—C6—C70.1 (8)
C11—Cu1—N1—C5177.3 (4)Cu1—N3—C6—C7175.2 (4)
Cu1i—Cu1—N1—C5151.3 (3)C5—N2—C6—N311.9 (9)
N3—Cu1—N1—C1168.7 (4)C5—N2—C6—C7167.2 (5)
O1—Cu1—N1—C13.5 (4)N3—C6—C7—C80.3 (9)
O2—Cu1—N1—C134.9 (6)N2—C6—C7—C8178.8 (5)
O5i—Cu1—N1—C194.0 (4)C6—C7—C8—C90.8 (10)
C11—Cu1—N1—C15.0 (5)C7—C8—C9—C100.8 (10)
Cu1i—Cu1—N1—C126.4 (5)C6—N3—C10—C90.1 (8)
N1—Cu1—N3—C614.8 (4)Cu1—N3—C10—C9175.5 (5)
O1—Cu1—N3—C6161.0 (6)C8—C9—C10—N30.4 (10)
O2—Cu1—N3—C6177.3 (4)Cu1—O2—C11—O16.3 (5)
O5i—Cu1—N3—C685.2 (4)Cu1—O2—C11—C12174.2 (4)
C11—Cu1—N3—C6177.0 (4)Cu1—O1—C11—O26.6 (5)
Cu1i—Cu1—N3—C6150.6 (3)Cu1—O1—C11—C12173.9 (4)
N1—Cu1—N3—C10170.1 (4)N3—Cu1—C11—O20.6 (4)
O1—Cu1—N3—C1023.9 (9)N1—Cu1—C11—O2157.5 (3)
O2—Cu1—N3—C107.5 (4)O1—Cu1—C11—O2173.4 (5)
O5i—Cu1—N3—C1090.0 (4)O5i—Cu1—C11—O299.5 (3)
C11—Cu1—N3—C107.8 (5)Cu1i—Cu1—C11—O293.3 (4)
Cu1i—Cu1—N3—C1024.5 (5)N3—Cu1—C11—O1172.8 (3)
N3—Cu1—O1—C1121.6 (9)N1—Cu1—C11—O115.9 (4)
N1—Cu1—O1—C11167.6 (3)O2—Cu1—C11—O1173.4 (5)
O2—Cu1—O1—C113.9 (3)O5i—Cu1—C11—O187.0 (3)
O5i—Cu1—O1—C1193.0 (3)Cu1i—Cu1—C11—O193.3 (4)
Cu1i—Cu1—O1—C1138.3 (2)O2—C11—C12—C170.2 (7)
N3—Cu1—O2—C11179.6 (3)O1—C11—C12—C17179.3 (5)
N1—Cu1—O2—C1147.1 (5)O2—C11—C12—C13179.6 (5)
O1—Cu1—O2—C113.9 (3)O1—C11—C12—C130.9 (7)
O5i—Cu1—O2—C1182.4 (3)C17—C12—C13—C140.1 (8)
Cu1i—Cu1—O2—C1138.8 (2)C11—C12—C13—C14179.6 (5)
O4—S1—O5—Cu1i157.2 (7)C12—C13—C14—C150.4 (8)
O4'—S1—O5—Cu1i174.2 (7)C13—C14—C15—C160.6 (8)
O3—S1—O5—Cu1i35.1 (5)C13—C14—C15—S1178.9 (4)
C15—S1—O5—Cu1i78.9 (4)O4—S1—C15—C1499.6 (7)
C5—N1—C1—C20.9 (8)O5—S1—C15—C14127.6 (5)
Cu1—N1—C1—C2176.9 (5)O4'—S1—C15—C14128.3 (8)
N1—C1—C2—C30.4 (10)O3—S1—C15—C1411.6 (6)
C1—C2—C3—C40.1 (10)O4—S1—C15—C1679.9 (7)
C2—C3—C4—C50.4 (9)O5—S1—C15—C1652.9 (5)
C1—N1—C5—N2178.8 (5)O4'—S1—C15—C1651.2 (8)
Cu1—N1—C5—N23.5 (7)O3—S1—C15—C16168.9 (5)
C1—N1—C5—C41.1 (7)C14—C15—C16—C170.5 (8)
Cu1—N1—C5—C4176.5 (4)S1—C15—C16—C17179.0 (4)
C6—N2—C5—N113.1 (9)C13—C12—C17—C160.0 (8)
C6—N2—C5—C4166.9 (5)C11—C12—C17—C16179.7 (5)
C3—C4—C5—N10.9 (8)C15—C16—C17—C120.2 (8)
Symmetry code: (i) x+1, y+1, z+1.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N2—H2N···O1W0.861.982.817 (11)165
N2—H2N···O1W0.862.132.857 (15)141
O1W—H1A···O4ii0.812.082.844 (12)158
O1W—H1B···O2Wiii0.831.662.349 (15)139
O1W—H1C···O4iv0.851.662.393 (15)142
O1W—H1C···O4iv0.851.952.773 (15)162
O1W—H1D···O2Wiii0.871.912.767 (18)171
O2W—H1W···O10.852.112.925 (10)160
O2W—H2W···O4v0.852.283.025 (17)147
O2W—H2W···O3v0.852.323.104 (12)153
Symmetry codes: (ii) x+1, y1, z1; (iii) x+1, y, z; (iv) x+1, y, z+1; (v) x, y+1, z+1.
 

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