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In the title compound, [Cu2(C8H4O5)2(C12H8N2)2(H2O)2]·3H2O, the Cu complex forms a centrosymmetric dimer with a Cu...Cu separation of 8.198 (3) Å. In the 5-hydroxy­isophthalate ligands, two carboxyl­ate groups coordinate two copper(II) cations in μ2-bridging bidentate coordination modes.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536804023190/cv6376sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536804023190/cv6376Isup2.hkl
Contains datablock I

CCDC reference: 252942

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](C-C) = 0.010 Å
  • Disorder in solvent or counterion
  • R factor = 0.084
  • wR factor = 0.172
  • Data-to-parameter ratio = 11.4

checkCIF/PLATON results

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Alert level C PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT302_ALERT_4_C Anion/Solvent Disorder ......................... 25.00 Perc. PLAT341_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 10
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 3 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 0 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 1 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: XP (Bruker, 2002); software used to prepare material for publication: SHELXTL (Bruker, 2002).

Di-µ-5-hydroxyisophthalato-bis[aqua(1,10-phenanthroline)copper(II)] trihydrate top
Crystal data top
[Cu2(C8H4O5)2(C12H8N2)2(H2O)2]·3H2OZ = 1
Mr = 937.79F(000) = 480
Triclinic, P1Dx = 1.652 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 7.2751 (10) ÅCell parameters from 1209 reflections
b = 10.4797 (14) Åθ = 2.9–23.3°
c = 12.7575 (17) ŵ = 1.21 mm1
α = 97.482 (2)°T = 293 K
β = 92.284 (2)°Prism, blue
γ = 101.475 (2)°0.25 × 0.16 × 0.10 mm
V = 942.9 (2) Å3
Data collection top
Bruker APEX area-detector
diffractometer
3383 independent reflections
Radiation source: fine-focus sealed tube3353 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.027
φ and ω scansθmax = 25.2°, θmin = 1.6°
Absorption correction: multi-scan
(SADABS; Bruker, 2002)
h = 88
Tmin = 0.752, Tmax = 0.889k = 1212
6956 measured reflectionsl = 1515
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)] = 0.084Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.172H atoms treated by a mixture of independent and constrained refinement
S = 1.34 w = 1/[σ2(Fo2) + (0.0361P)2 + 4.7073P]
where P = (Fo2 + 2Fc2)/3
3383 reflections(Δ/σ)max < 0.001
296 parametersΔρmax = 0.91 e Å3
6 restraintsΔρmin = 1.16 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)
Cu10.56165 (10)0.94671 (7)0.77592 (6)0.0210 (2)
O10.8321 (6)1.0023 (5)0.6939 (4)0.0343 (11)
O21.1211 (6)1.1180 (4)0.7375 (4)0.0398 (12)
O31.3257 (7)0.9752 (4)1.0839 (3)0.0317 (11)
O41.3084 (7)0.7613 (4)1.0883 (4)0.0372 (12)
O50.9753 (7)0.5502 (4)0.7323 (4)0.0371 (12)
H51.01700.49820.76470.056*
O60.4817 (6)1.1077 (4)0.7444 (3)0.0286 (10)
H6B0.36741.09810.74730.043*
H6C0.53431.15330.79840.043*
O80.7893 (16)0.8366 (9)0.4906 (7)0.040 (2)0.50
N10.5685 (7)0.7675 (5)0.8149 (4)0.0243 (11)
N20.4239 (7)0.8399 (5)0.6453 (4)0.0244 (11)
C10.6418 (9)0.7354 (7)0.9015 (5)0.0326 (15)
H10.69870.80210.95510.039*
C20.6371 (10)0.6045 (7)0.9156 (6)0.0381 (17)
H20.68930.58470.97760.046*
C30.5555 (11)0.5075 (7)0.8375 (6)0.0431 (18)
H30.55270.42040.84610.052*
C40.4753 (9)0.5360 (6)0.7443 (6)0.0340 (16)
C50.3827 (11)0.4412 (7)0.6579 (6)0.0441 (19)
H5A0.37490.35210.66110.053*
C60.3073 (11)0.4786 (7)0.5726 (6)0.0428 (18)
H6A0.24650.41460.51810.051*
C70.3173 (9)0.6146 (7)0.5627 (5)0.0332 (15)
C80.2417 (11)0.6603 (8)0.4761 (6)0.0444 (19)
H80.17900.60100.41920.053*
C90.2599 (10)0.7912 (8)0.4750 (5)0.0410 (18)
H90.21150.82230.41700.049*
C100.3515 (9)0.8789 (7)0.5615 (5)0.0333 (15)
H100.36210.96860.56010.040*
C110.4084 (9)0.7087 (6)0.6452 (5)0.0267 (14)
C120.4873 (8)0.6696 (6)0.7367 (5)0.0234 (13)
C130.9937 (9)1.0161 (6)0.7352 (5)0.0279 (14)
C141.0433 (8)0.9042 (6)0.7871 (5)0.0229 (13)
C151.1397 (9)0.9297 (6)0.8854 (5)0.0251 (13)
H151.17891.01610.91820.030*
C161.1785 (8)0.8275 (6)0.9358 (5)0.0223 (12)
C171.2784 (9)0.8555 (6)1.0440 (5)0.0251 (13)
C181.1244 (8)0.6993 (6)0.8857 (5)0.0248 (13)
H181.15100.63050.91890.030*
C191.0301 (9)0.6734 (6)0.7859 (5)0.0258 (13)
C200.9855 (9)0.7759 (6)0.7379 (5)0.0259 (13)
H200.91680.75830.67280.031*
H8B0.847 (18)0.852 (12)0.440 (6)0.039*0.50
H8C0.794 (19)0.889 (9)0.541 (6)0.039*0.50
O70.0422 (9)0.3563 (5)0.8358 (5)0.0556 (16)
H7B0.062 (10)0.293 (5)0.799 (5)0.03 (2)*
H7C0.060 (6)0.331 (7)0.858 (6)0.04 (2)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Cu10.0225 (4)0.0163 (4)0.0236 (4)0.0029 (3)0.0021 (3)0.0035 (3)
O10.023 (2)0.041 (3)0.042 (3)0.005 (2)0.000 (2)0.017 (2)
O20.022 (2)0.027 (3)0.070 (4)0.000 (2)0.002 (2)0.019 (2)
O30.050 (3)0.021 (2)0.022 (2)0.007 (2)0.008 (2)0.0001 (18)
O40.049 (3)0.021 (2)0.040 (3)0.006 (2)0.013 (2)0.005 (2)
O50.050 (3)0.020 (2)0.037 (3)0.007 (2)0.006 (2)0.006 (2)
O60.028 (2)0.022 (2)0.036 (3)0.0056 (18)0.0068 (19)0.0055 (19)
O80.069 (7)0.028 (5)0.022 (5)0.007 (5)0.005 (5)0.001 (4)
N10.021 (3)0.026 (3)0.027 (3)0.003 (2)0.005 (2)0.006 (2)
N20.024 (3)0.023 (3)0.024 (3)0.000 (2)0.002 (2)0.002 (2)
C10.034 (4)0.036 (4)0.030 (4)0.005 (3)0.004 (3)0.012 (3)
C20.044 (4)0.043 (4)0.036 (4)0.020 (3)0.009 (3)0.021 (3)
C30.047 (4)0.033 (4)0.057 (5)0.017 (3)0.021 (4)0.017 (4)
C40.032 (4)0.027 (4)0.045 (4)0.008 (3)0.015 (3)0.007 (3)
C50.057 (5)0.024 (4)0.050 (5)0.007 (3)0.016 (4)0.001 (3)
C60.045 (4)0.033 (4)0.044 (4)0.001 (3)0.003 (3)0.005 (3)
C70.034 (4)0.032 (4)0.031 (4)0.004 (3)0.008 (3)0.001 (3)
C80.045 (5)0.044 (5)0.036 (4)0.001 (4)0.004 (3)0.009 (3)
C90.044 (4)0.057 (5)0.022 (3)0.009 (4)0.006 (3)0.006 (3)
C100.036 (4)0.030 (4)0.033 (4)0.006 (3)0.001 (3)0.005 (3)
C110.028 (3)0.020 (3)0.031 (3)0.004 (3)0.006 (3)0.001 (3)
C120.024 (3)0.019 (3)0.028 (3)0.006 (2)0.011 (2)0.000 (2)
C130.029 (3)0.031 (3)0.025 (3)0.011 (3)0.000 (3)0.003 (3)
C140.018 (3)0.021 (3)0.029 (3)0.003 (2)0.006 (2)0.003 (2)
C150.030 (3)0.020 (3)0.024 (3)0.005 (3)0.002 (3)0.000 (2)
C160.020 (3)0.022 (3)0.024 (3)0.004 (2)0.003 (2)0.002 (2)
C170.027 (3)0.025 (3)0.024 (3)0.008 (3)0.005 (3)0.002 (3)
C180.029 (3)0.019 (3)0.028 (3)0.005 (3)0.006 (3)0.003 (2)
C190.025 (3)0.020 (3)0.032 (3)0.005 (2)0.009 (3)0.001 (3)
C200.029 (3)0.027 (3)0.021 (3)0.005 (3)0.002 (2)0.002 (3)
O70.065 (4)0.027 (3)0.078 (4)0.009 (3)0.029 (4)0.011 (3)
Geometric parameters (Å, º) top
Cu1—O3i1.942 (4)C4—C51.430 (10)
Cu1—O61.974 (4)C5—C61.337 (11)
Cu1—N21.992 (5)C5—H5A0.9300
Cu1—N12.013 (5)C6—C71.434 (10)
Cu1—O12.274 (5)C6—H6A0.9300
O1—C131.243 (8)C7—C111.391 (9)
O2—C131.263 (8)C7—C81.396 (10)
O3—C171.265 (7)C8—C91.353 (11)
O3—Cu1i1.942 (4)C8—H80.9300
O4—C171.250 (7)C9—C101.393 (9)
O5—C191.355 (7)C9—H90.9300
O5—H50.8200C10—H100.9300
O6—H6B0.8200C11—C121.423 (9)
O6—H6C0.8185C13—C141.515 (9)
O8—H8B0.80 (3)C14—C151.380 (8)
O8—H8C0.79 (3)C14—C201.383 (8)
N1—C11.319 (8)C15—C161.387 (8)
N1—C121.356 (8)C15—H150.9300
N2—C101.321 (8)C16—C181.384 (8)
N2—C111.357 (8)C16—C171.500 (8)
C1—C21.400 (9)C18—C191.390 (9)
C1—H10.9300C18—H180.9300
C2—C31.351 (11)C19—C201.389 (9)
C2—H20.9300C20—H200.9300
C3—C41.397 (11)O7—H7B0.81 (3)
C3—H30.9300O7—H7C0.81 (3)
C4—C121.402 (9)
O3i—Cu1—O694.36 (18)C11—C7—C6118.1 (6)
O3i—Cu1—N2169.7 (2)C8—C7—C6124.9 (7)
O6—Cu1—N292.6 (2)C9—C8—C7119.9 (7)
O3i—Cu1—N189.20 (19)C9—C8—H8120.0
O6—Cu1—N1164.33 (19)C7—C8—H8120.0
N2—Cu1—N182.1 (2)C8—C9—C10119.5 (7)
O3i—Cu1—O194.25 (19)C8—C9—H9120.3
O6—Cu1—O190.84 (18)C10—C9—H9120.3
N2—Cu1—O193.33 (19)N2—C10—C9122.6 (6)
N1—Cu1—O1104.13 (18)N2—C10—H10118.7
C13—O1—Cu1125.5 (4)C9—C10—H10118.7
C17—O3—Cu1i129.8 (4)N2—C11—C7123.3 (6)
C19—O5—H5109.5N2—C11—C12116.4 (5)
Cu1—O6—H6B109.5C7—C11—C12120.3 (6)
Cu1—O6—H6C94.6N1—C12—C4123.1 (6)
H6B—O6—H6C109.6N1—C12—C11116.5 (5)
H8B—O8—H8C122 (6)C4—C12—C11120.3 (6)
C1—N1—C12118.4 (6)O1—C13—O2124.5 (6)
C1—N1—Cu1129.5 (5)O1—C13—C14118.4 (6)
C12—N1—Cu1112.1 (4)O2—C13—C14117.0 (5)
C10—N2—C11117.7 (5)C15—C14—C20119.9 (6)
C10—N2—Cu1129.4 (4)C15—C14—C13120.1 (5)
C11—N2—Cu1112.9 (4)C20—C14—C13120.0 (6)
N1—C1—C2122.3 (7)C14—C15—C16120.6 (6)
N1—C1—H1118.8C14—C15—H15119.7
C2—C1—H1118.8C16—C15—H15119.7
C3—C2—C1119.0 (7)C18—C16—C15119.6 (6)
C3—C2—H2120.5C18—C16—C17120.0 (5)
C1—C2—H2120.5C15—C16—C17120.3 (5)
C2—C3—C4121.1 (7)O4—C17—O3124.8 (6)
C2—C3—H3119.5O4—C17—C16118.9 (5)
C4—C3—H3119.5O3—C17—C16116.3 (5)
C3—C4—C12116.1 (7)C16—C18—C19120.0 (6)
C3—C4—C5125.6 (7)C16—C18—H18120.0
C12—C4—C5118.3 (7)C19—C18—H18120.0
C6—C5—C4121.0 (7)O5—C19—C20117.3 (6)
C6—C5—H5A119.5O5—C19—C18122.8 (6)
C4—C5—H5A119.5C20—C19—C18119.9 (6)
C5—C6—C7121.9 (7)C14—C20—C19120.0 (6)
C5—C6—H6A119.0C14—C20—H20120.0
C7—C6—H6A119.0C19—C20—H20120.0
C11—C7—C8117.0 (6)H7B—O7—H7C104 (8)
Symmetry code: (i) x+2, y+2, z+2.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O5—H5···O7ii0.821.882.673 (8)164
O6—H6B···O2iii0.821.852.645 (6)164
O6—H6C···O4i0.821.822.630 (6)168
O6—H6C···O3i0.822.462.872 (6)112
O8—H8B···O2iv0.80 (3)2.35 (7)3.084 (11)155 (14)
O8—H8C···O10.79 (3)2.12 (4)2.896 (10)168 (15)
O7—H7B···O2v0.81 (3)2.03 (3)2.820 (8)167 (8)
O7—H7C···O4vi0.81 (3)2.06 (3)2.867 (8)171 (7)
Symmetry codes: (i) x+2, y+2, z+2; (ii) x+1, y, z; (iii) x1, y, z; (iv) x+2, y+2, z+1; (v) x1, y1, z; (vi) x+1, y+1, z+2.
 

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