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In the title compound, [Cu3(C10H9N3)3(C7H3O6S)2]·3H2O, [Cu3(ssal)2(dpa)3] units (dpa is 2,2′-dipyridylamine and ssal is 5-sulfonatosalicylate) are found, which consist of one crystallographically independent ssal anion, and two each of crystallographically independent dpa ligands and Cu atoms, the unit lying on a twofold rotation axis. One Cu atom is four-coordinated by one dpa ligand and one ssal anion within a square-planar geometry, whereas the second Cu atom is coordinated by one dpa ligand and two ssal anions which are related by symmetry. The first Cu atom has one longer contact to one O atom of a symmetry-related sulfonate group and is, therefore, five-coordinated within a distorted square-pyramidal coordination. The [Cu3(ssal)2(dpa)3] units are connected via the sulfonate groups into layers which are parallel to the ab plane. These layers are further connected by O—H...O and N—H...O hydrogen bonding via the water molecules.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536804032908/nc6010sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536804032908/nc6010Isup2.hkl
Contains datablock I

CCDC reference: 262290

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](C-C) = 0.005 Å
  • H-atom completeness 90%
  • R factor = 0.042
  • wR factor = 0.102
  • Data-to-parameter ratio = 14.7

checkCIF/PLATON results

No syntax errors found



Alert level A PLAT306_ALERT_2_A Isolated Oxygen Atom (H-atoms Missing ?) ....... O8
Author Response: see _publ_section_exptl_refinement.

Alert level C PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings Differ .... ? PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT068_ALERT_1_C Reported F000 Differs from Calcd (or Missing)... ? PLAT199_ALERT_1_C Check the Reported cell_measurement_temperature 293 PLAT200_ALERT_1_C Check the Reported cell_ambient_temperature .... 293 PLAT250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor .... 2.03 PLAT716_ALERT_1_C H...A Unknown or Inconsistent Label .......... ? PLAT716_ALERT_1_C H...A Unknown or Inconsistent Label .......... ?
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:C44 H39 Cu3 N9 O15 S2 Atom count from the _atom_site data: C44 H35 Cu3 N9 O15 S2 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 C44 H39 Cu3 N9 O15 S2 TEST: Compare cell contents of formula and atom_site data atom Z*formula cif sites diff C 176.00 176.00 0.00 H 156.00 140.00 16.00 Cu 12.00 12.00 0.00 N 36.00 36.00 0.00 O 60.00 60.00 0.00 S 8.00 8.00 0.00
1 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 8 ALERT level C = Check and explain 3 ALERT level G = General alerts; check 9 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 3 ALERT type 2 Indicator that the structure model may be wrong or deficient 0 ALERT type 3 Indicator that the structure quality may be low 0 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: SMART (Bruker, 1997); cell refinement: SMART; data reduction: SHELXTL (Bruker, 1997); 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).

Poly[[tris(di-2-pyridylamine)bis(µ-5-sulfonatosalicylato)tricopper(II)] trihydrate] top
Crystal data top
[Cu3(C10H9N3)3(C7H3O6S)2]·3H2OF(000) = 2420
Mr = 1188.58Dx = 1.748 Mg m3
Monoclinic, C2/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2ycCell parameters from 3596 reflections
a = 11.3447 (10) Åθ = 4.8–53.8°
b = 13.4618 (11) ŵ = 1.58 mm1
c = 29.910 (3) ÅT = 293 K
β = 98.650 (2)°Plate, green
V = 4516.0 (7) Å30.51 × 0.32 × 0.13 mm
Z = 4
Data collection top
Bruker SMART CCD area-detector
diffractometer
4979 independent reflections
Radiation source: fine-focus sealed tube3744 reflections with I > 2s˘I)
Graphite monochromatorRint = 0.087
φ and ω scansθmax = 27.1°, θmin = 2.4°
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
h = 1413
Tmin = 0.550, Tmax = 0.816k = 917
13200 measured reflectionsl = 3738
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)] = 0.042Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.102H-atom parameters constrained
S = 0.96 w = 1/[σ2(Fo2) + (0.0385P)2]
where P = (Fo2 + 2Fc2)/3
4979 reflections(Δ/σ)max < 0.001
338 parametersΔρmax = 0.58 e Å3
3 restraintsΔρmin = 0.37 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*/Ueq
Cu10.00000.35206 (3)0.25000.02643 (15)
Cu20.16085 (3)0.40996 (2)0.118533 (12)0.02849 (12)
S10.01886 (7)0.10251 (5)0.12587 (3)0.02966 (19)
N10.2139 (2)0.52019 (17)0.16044 (9)0.0282 (6)
N20.1294 (3)0.64202 (18)0.10944 (10)0.0395 (7)
N30.1572 (2)0.50165 (18)0.06608 (9)0.0333 (6)
N40.0774 (2)0.45240 (17)0.29276 (8)0.0267 (6)
N50.00000.5910 (3)0.25000.0339 (9)
O10.1190 (2)0.34033 (14)0.17079 (7)0.0326 (5)
O20.00318 (19)0.24699 (14)0.20558 (7)0.0303 (5)
O30.0995 (2)0.30461 (15)0.07958 (7)0.0388 (6)
O40.1421 (2)0.13190 (16)0.11576 (9)0.0494 (7)
O50.0535 (2)0.15779 (14)0.09863 (8)0.0403 (6)
O60.0260 (3)0.10788 (16)0.17344 (8)0.0519 (7)
O70.00000.2040 (3)0.25000.0934 (18)
O80.1678 (4)0.2745 (3)0.04190 (13)0.1071 (13)
C10.0554 (3)0.2637 (2)0.17188 (10)0.0248 (6)
C20.0398 (3)0.19217 (19)0.13439 (10)0.0239 (6)
C30.0620 (3)0.2180 (2)0.09111 (10)0.0288 (7)
C40.0437 (3)0.1432 (2)0.05734 (10)0.0376 (8)
H40.05250.15890.02770.045*
C50.0137 (3)0.0488 (2)0.06750 (11)0.0353 (8)
H50.00410.00080.04490.042*
C60.0026 (3)0.0231 (2)0.11085 (10)0.0277 (7)
C70.0067 (3)0.0955 (2)0.14363 (10)0.0258 (6)
H70.00930.07970.17240.031*
C80.2730 (3)0.4974 (2)0.20185 (11)0.0330 (7)
H80.29820.43230.20750.040*
C90.2971 (3)0.5651 (3)0.23552 (12)0.0383 (8)
H90.34000.54710.26330.046*
C100.2567 (3)0.6615 (3)0.22775 (12)0.0420 (9)
H100.26850.70840.25080.050*
C110.1995 (3)0.6866 (2)0.18612 (11)0.0352 (8)
H110.17200.75110.18030.042*
C120.1826 (3)0.6146 (2)0.15219 (10)0.0272 (7)
C130.1395 (3)0.5992 (2)0.06846 (11)0.0324 (7)
C140.1298 (3)0.6605 (2)0.03053 (12)0.0457 (9)
H140.11670.72840.03300.055*
C150.1396 (4)0.6193 (3)0.00977 (13)0.0580 (11)
H150.13210.65870.03560.070*
C160.1610 (4)0.5187 (3)0.01274 (12)0.0558 (11)
H160.17020.48950.04020.067*
C170.1682 (4)0.4634 (3)0.02588 (12)0.0496 (10)
H170.18150.39540.02400.059*
C180.1459 (3)0.4196 (2)0.33111 (11)0.0350 (8)
H180.15910.35160.33430.042*
C190.1956 (3)0.4793 (3)0.36465 (12)0.0427 (9)
H190.24340.45310.38990.051*
C200.1746 (3)0.5797 (3)0.36108 (12)0.0437 (9)
H200.20550.62220.38440.052*
C210.1083 (3)0.6160 (2)0.32310 (12)0.0370 (8)
H210.09420.68380.32000.044*
C220.0609 (3)0.5503 (2)0.28834 (10)0.0271 (7)
H2A0.124 (3)0.7017 (8)0.1109 (12)0.050*
H5A0.00000.6503 (8)0.25000.050*
H7A0.001 (4)0.176 (3)0.2738 (8)0.080*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Cu10.0433 (3)0.0169 (3)0.0196 (3)0.0000.0064 (2)0.000
Cu20.0455 (3)0.01585 (19)0.0253 (2)0.00287 (16)0.00905 (17)0.00065 (14)
S10.0413 (5)0.0144 (4)0.0348 (5)0.0011 (3)0.0107 (4)0.0002 (3)
N10.0352 (15)0.0190 (13)0.0312 (15)0.0027 (11)0.0081 (12)0.0003 (10)
N20.061 (2)0.0188 (14)0.0396 (17)0.0081 (14)0.0112 (14)0.0012 (12)
N30.0524 (18)0.0207 (13)0.0284 (15)0.0000 (12)0.0115 (13)0.0023 (11)
N40.0341 (15)0.0210 (13)0.0257 (14)0.0014 (11)0.0065 (11)0.0022 (10)
N50.047 (2)0.0189 (19)0.036 (2)0.0000.0059 (18)0.000
O10.0477 (14)0.0247 (11)0.0271 (12)0.0146 (10)0.0117 (10)0.0050 (9)
O20.0517 (14)0.0197 (10)0.0222 (11)0.0054 (9)0.0137 (10)0.0035 (8)
O30.0718 (17)0.0196 (11)0.0250 (12)0.0121 (11)0.0074 (11)0.0008 (9)
O40.0413 (14)0.0278 (13)0.081 (2)0.0033 (11)0.0156 (13)0.0060 (12)
O50.0547 (15)0.0201 (11)0.0501 (15)0.0083 (10)0.0212 (12)0.0009 (10)
O60.095 (2)0.0260 (12)0.0345 (14)0.0022 (12)0.0078 (14)0.0052 (10)
O70.222 (6)0.024 (2)0.047 (3)0.0000.061 (3)0.000
O80.136 (4)0.105 (3)0.081 (3)0.003 (2)0.018 (2)0.021 (2)
C10.0347 (17)0.0167 (14)0.0224 (16)0.0026 (12)0.0026 (13)0.0021 (11)
C20.0332 (17)0.0153 (14)0.0234 (15)0.0002 (12)0.0053 (13)0.0026 (11)
C30.048 (2)0.0167 (15)0.0224 (16)0.0015 (13)0.0055 (14)0.0012 (11)
C40.070 (3)0.0238 (17)0.0190 (16)0.0045 (16)0.0079 (16)0.0005 (12)
C50.059 (2)0.0212 (16)0.0259 (17)0.0045 (15)0.0057 (15)0.0071 (13)
C60.0377 (18)0.0160 (14)0.0288 (17)0.0015 (12)0.0031 (14)0.0007 (12)
C70.0353 (17)0.0186 (15)0.0245 (16)0.0034 (12)0.0080 (13)0.0015 (12)
C80.0327 (18)0.0272 (17)0.039 (2)0.0034 (13)0.0063 (15)0.0003 (14)
C90.0351 (19)0.046 (2)0.0331 (19)0.0099 (16)0.0024 (15)0.0034 (15)
C100.046 (2)0.038 (2)0.043 (2)0.0136 (16)0.0093 (17)0.0192 (16)
C110.041 (2)0.0224 (16)0.044 (2)0.0058 (14)0.0116 (16)0.0073 (14)
C120.0325 (17)0.0186 (15)0.0317 (18)0.0031 (12)0.0090 (14)0.0002 (12)
C130.0416 (19)0.0227 (16)0.0336 (19)0.0031 (14)0.0079 (15)0.0032 (13)
C140.073 (3)0.0255 (18)0.040 (2)0.0064 (17)0.0111 (19)0.0090 (15)
C150.091 (3)0.045 (2)0.037 (2)0.003 (2)0.009 (2)0.0204 (18)
C160.102 (4)0.041 (2)0.028 (2)0.000 (2)0.021 (2)0.0013 (16)
C170.089 (3)0.0265 (19)0.037 (2)0.0011 (18)0.024 (2)0.0020 (15)
C180.042 (2)0.0307 (18)0.0318 (19)0.0057 (14)0.0036 (15)0.0013 (14)
C190.037 (2)0.059 (2)0.0303 (19)0.0022 (17)0.0020 (15)0.0013 (16)
C200.046 (2)0.052 (2)0.033 (2)0.0100 (17)0.0059 (16)0.0150 (16)
C210.048 (2)0.0246 (17)0.039 (2)0.0053 (15)0.0096 (16)0.0073 (14)
C220.0320 (17)0.0210 (15)0.0296 (17)0.0026 (13)0.0095 (13)0.0024 (12)
Geometric parameters (Å, º) top
Cu1—O21.9447 (19)C2—C31.400 (4)
Cu1—O2i1.9447 (19)C3—C41.420 (4)
Cu1—N41.973 (2)C4—C51.362 (4)
Cu1—N4i1.973 (2)C4—H40.9300
Cu2—O31.900 (2)C5—C61.381 (4)
Cu2—O11.942 (2)C5—H50.9300
Cu2—N11.977 (2)C6—C71.375 (4)
Cu2—N31.992 (2)C7—H70.9300
Cu2—O4ii2.318 (2)C8—C91.355 (4)
S1—O61.439 (3)C8—H80.9300
S1—O41.441 (2)C9—C101.384 (5)
S1—O51.447 (2)C9—H90.9300
S1—C61.767 (3)C10—C111.358 (5)
N1—C121.333 (4)C10—H100.9300
N1—C81.352 (4)C11—C121.396 (4)
N2—C131.375 (4)C11—H110.9300
N2—C121.380 (4)C13—C141.393 (4)
N2—H2A0.808 (10)C14—C151.347 (5)
N3—C171.331 (4)C14—H140.9300
N3—C131.332 (4)C15—C161.382 (5)
N4—C221.335 (3)C15—H150.9300
N4—C181.359 (4)C16—C171.367 (5)
N5—C221.362 (3)C16—H160.9300
N5—C22i1.362 (3)C17—H170.9300
N5—H5A0.798 (10)C18—C191.341 (4)
O1—C11.262 (3)C18—H180.9300
O2—C11.264 (3)C19—C201.374 (5)
O3—C31.305 (3)C19—H190.9300
O4—Cu2iii2.318 (2)C20—C211.356 (5)
O7—H7A0.81 (3)C20—H200.9300
C1—C21.468 (4)C21—C221.408 (4)
C2—C71.394 (4)C21—H210.9300
O2—Cu1—O2i86.67 (12)C4—C5—H5119.5
O2—Cu1—N4152.71 (9)C6—C5—H5119.5
O2i—Cu1—N496.15 (9)C7—C6—C5119.1 (3)
O2—Cu1—N4i96.15 (9)C7—C6—S1119.8 (2)
O2i—Cu1—N4i152.71 (9)C5—C6—S1120.8 (2)
N4—Cu1—N4i93.59 (14)C6—C7—C2121.0 (3)
O3—Cu2—O191.27 (8)C6—C7—H7119.5
O3—Cu2—N1176.10 (10)C2—C7—H7119.5
O1—Cu2—N186.56 (9)N1—C8—C9123.1 (3)
O3—Cu2—N390.99 (10)N1—C8—H8118.5
O1—Cu2—N3162.68 (10)C9—C8—H8118.5
N1—Cu2—N390.14 (10)C8—C9—C10118.7 (3)
O3—Cu2—O4ii93.59 (9)C8—C9—H9120.6
O1—Cu2—O4ii105.37 (9)C10—C9—H9120.6
N1—Cu2—O4ii90.10 (9)C11—C10—C9119.3 (3)
N3—Cu2—O4ii91.62 (10)C11—C10—H10120.4
O6—S1—O4112.41 (16)C9—C10—H10120.4
O6—S1—O5112.62 (15)C10—C11—C12119.2 (3)
O4—S1—O5110.84 (14)C10—C11—H11120.4
O6—S1—C6105.34 (14)C12—C11—H11120.4
O4—S1—C6110.17 (14)N1—C12—N2119.6 (3)
O5—S1—C6105.03 (13)N1—C12—C11121.6 (3)
C12—N1—C8117.9 (3)N2—C12—C11118.7 (3)
C12—N1—Cu2123.4 (2)N3—C13—N2119.6 (3)
C8—N1—Cu2118.2 (2)N3—C13—C14122.3 (3)
C13—N2—C12129.1 (3)N2—C13—C14118.1 (3)
C13—N2—H2A119 (3)C15—C14—C13118.6 (3)
C12—N2—H2A104 (3)C15—C14—H14120.7
C17—N3—C13117.7 (3)C13—C14—H14120.7
C17—N3—Cu2118.5 (2)C14—C15—C16120.0 (3)
C13—N3—Cu2123.7 (2)C14—C15—H15120.0
C22—N4—C18117.3 (3)C16—C15—H15120.0
C22—N4—Cu1124.7 (2)C17—C16—C15118.0 (3)
C18—N4—Cu1117.8 (2)C17—C16—H16121.0
C22—N5—C22i132.5 (4)C15—C16—H16121.0
C22—N5—H5A113.75 (18)N3—C17—C16123.4 (3)
C22i—N5—H5A113.75 (18)N3—C17—H17118.3
C1—O1—Cu2128.70 (19)C16—C17—H17118.3
C1—O2—Cu1118.33 (17)C19—C18—N4124.0 (3)
C3—O3—Cu2127.49 (19)C19—C18—H18118.0
S1—O4—Cu2iii146.74 (14)N4—C18—H18118.0
O2—C1—O1120.3 (3)C18—C19—C20118.8 (3)
O2—C1—C2118.4 (2)C18—C19—H19120.6
O1—C1—C2121.3 (3)C20—C19—H19120.6
C7—C2—C3120.5 (3)C21—C20—C19119.2 (3)
C7—C2—C1117.8 (3)C21—C20—H20120.4
C3—C2—C1121.7 (3)C19—C20—H20120.4
O3—C3—C2125.3 (3)C20—C21—C22119.6 (3)
O3—C3—C4117.7 (3)C20—C21—H21120.2
C2—C3—C4117.0 (3)C22—C21—H21120.2
C5—C4—C3121.2 (3)N4—C22—N5121.8 (3)
C5—C4—H4119.4N4—C22—C21121.0 (3)
C3—C4—H4119.4N5—C22—C21117.2 (3)
C4—C5—C6121.1 (3)
Symmetry codes: (i) x, y, z+1/2; (ii) x+1/2, y+1/2, z; (iii) x1/2, y1/2, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N2—H2A···O5iv0.81 (1)2.06 (2)2.833 (3)159 (4)
N5—H5A···O7iv0.80 (1)1.96 (1)2.759 (5)180 (1)
O7—H7A···O6i0.81 (3)1.88 (3)2.685 (3)172 (5)
O8···O8v??2.965 (8)?
O8···O4??2.908 (4)?
Symmetry codes: (i) x, y, z+1/2; (iv) x, y+1, z; (v) x1/2, y1/2, z.
 

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