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In the title compound, {[Cu24-C5H6O4)22-C14H16N2)]·2CH3CN}n, the Cu2 dinuclear units are connected by glutartate ligands, forming one-dimensional double chains. These chains, are in turn bridged by 1,4-bis­(pyridin-4-yl)butane ligands to form a two-dimensional layer structure parallel to (112). The carboxyl­ate groups of the glutarate ligand bridge two copper(II) ions, forming a paddle-wheel-type Cu2(CO2)4 dinuclear secondary building unit. A crystallographic inversion centre is located midway between two CuII ions, with a Cu...Cu distance of 2.639 (3) Å. The coordination geometry of the unique CuII ion is slightly disorted square pyramidal, formed by four equatorial carboxyl­ate O atoms and an axial pyridyl N atom.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S2414314617014481/lh4026sup1.cif
Contains datablock I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2414314617014481/lh4026Isup2.hkl
Contains datablock I

CCDC reference: 1578612

Key indicators

  • Single-crystal X-ray study
  • T = 170 K
  • Mean [sigma](C-C) = 0.007 Å
  • R factor = 0.047
  • wR factor = 0.108
  • Data-to-parameter ratio = 15.6

checkCIF/PLATON results

No syntax errors found



Alert level C PLAT029_ALERT_3_C _diffrn_measured_fraction_theta_full value Low . 0.977 Note PLAT094_ALERT_2_C Ratio of Maximum / Minimum Residual Density .... 2.49 Report PLAT241_ALERT_2_C High 'MainMol' Ueq as Compared to Neighbors of C36 Check PLAT244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors of C1S Check PLAT341_ALERT_3_C Low Bond Precision on C-C Bonds ............... 0.00708 Ang. PLAT601_ALERT_2_C Structure Contains Solvent Accessible VOIDS of . 36 Ang3 PLAT911_ALERT_3_C Missing # FCF Refl Between THmin & STh/L= 0.600 65 Report
Alert level G PLAT004_ALERT_5_G Polymeric Structure Found with Maximum Dimension 2 Info PLAT042_ALERT_1_G Calc. and Reported MoietyFormula Strings Differ Please Check PLAT045_ALERT_1_G Calculated and Reported Z Differ by a Factor ... 2.00 Check PLAT154_ALERT_1_G The s.u.'s on the Cell Angles are Equal ..(Note) 0.002 Degree PLAT720_ALERT_4_G Number of Unusual/Non-Standard Labels .......... 3 Note PLAT764_ALERT_4_G Overcomplete CIF Bond List Detected (Rep/Expd) . 1.17 Ratio PLAT910_ALERT_3_G Missing # of FCF Reflection(s) Below Theta(Min). 1 Note PLAT912_ALERT_4_G Missing # of FCF Reflections Above STh/L= 0.600 25 Note PLAT933_ALERT_2_G Number of OMIT Records in Embedded .res File ... 10 Note PLAT978_ALERT_2_G Number C-C Bonds with Positive Residual Density. 1 Info
0 ALERT level A = Most likely a serious problem - resolve or explain 0 ALERT level B = A potentially serious problem, consider carefully 7 ALERT level C = Check. Ensure it is not caused by an omission or oversight 10 ALERT level G = General information/check it is not something unexpected 3 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 5 ALERT type 2 Indicator that the structure model may be wrong or deficient 4 ALERT type 3 Indicator that the structure quality may be low 4 ALERT type 4 Improvement, methodology, query or suggestion 1 ALERT type 5 Informative message, check

Computing details top

Data collection: SMART (Bruker, 1997); cell refinement: SAINT (Bruker, 1997); data reduction: SAINT (Bruker, 1997); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL2013 (Sheldrick, 2015); molecular graphics: DIAMOND (Brandenburg & Berndt, 1998); software used to prepare material for publication: SHELXTL (Sheldrick, 2008).

Poly[[[µ2-1,4-bis(pyridin-4-yl)butane]bis(µ4-pentanedioato)dicopper(II)] acetonitrile disolvate] top
Crystal data top
[Cu2(C5H6O4)2(C14H16N2)].2C2H3NZ = 1
Mr = 681.67F(000) = 352
Triclinic, P1Dx = 1.452 Mg m3
a = 7.7525 (11) ÅMo Kα radiation, λ = 0.71073 Å
b = 7.9962 (11) ÅCell parameters from 2966 reflections
c = 12.8132 (18) Åθ = 2.2–26.2°
α = 87.867 (2)°µ = 1.42 mm1
β = 81.875 (2)°T = 170 K
γ = 82.674 (2)°Block, blue
V = 779.76 (19) Å30.21 × 0.10 × 0.07 mm
Data collection top
Bruker APEX CCD
diffractometer
1863 reflections with I > 2σ(I)
φ and ω scansRint = 0.062
Absorption correction: multi-scan
(SADABS; Bruker, 1997)
θmax = 26.0°, θmin = 2.6°
Tmin = 0.804, Tmax = 0.910h = 99
4341 measured reflectionsk = 99
2979 independent reflectionsl = 1511
Refinement top
Refinement on F20 restraints
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.047H-atom parameters constrained
wR(F2) = 0.108 w = 1/[σ2(Fo2) + (0.0347P)2]
where P = (Fo2 + 2Fc2)/3
S = 0.89(Δ/σ)max = 0.002
2979 reflectionsΔρmax = 0.95 e Å3
191 parametersΔρmin = 0.38 e Å3
Special details top

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Cu10.62490 (7)0.51464 (6)0.92000 (4)0.0290 (2)
O110.5339 (4)0.3241 (4)0.8619 (2)0.0412 (8)
O120.6750 (4)0.7057 (4)1.0021 (2)0.0404 (8)
O210.7596 (4)0.3508 (4)1.0043 (2)0.0404 (8)
O220.4478 (4)0.6742 (4)0.8592 (2)0.0381 (8)
N310.8414 (5)0.5371 (4)0.7959 (3)0.0331 (9)
C110.4123 (6)0.2480 (5)0.9120 (4)0.0306 (10)
C120.3767 (6)0.0878 (5)0.8647 (4)0.0380 (11)
H12A0.47350.00190.87520.046*
H12B0.37880.10670.78770.046*
C130.2032 (5)0.0246 (5)0.9092 (4)0.0347 (11)
H13A0.19650.01250.98680.042*
H13B0.10510.10950.89370.042*
C210.7012 (6)0.2860 (5)1.0915 (4)0.0307 (10)
C220.8184 (6)0.1436 (5)1.1359 (3)0.0343 (11)
H22A0.78900.13891.21360.041*
H22B0.94240.16501.11890.041*
C311.0050 (6)0.4805 (5)0.8086 (3)0.0336 (11)
H311.02500.42520.87350.040*
C321.1470 (6)0.4962 (6)0.7344 (4)0.0377 (11)
H321.26130.45010.74750.045*
C331.1231 (6)0.5799 (6)0.6399 (4)0.0396 (12)
C340.9544 (6)0.6400 (7)0.6260 (4)0.0554 (15)
H340.93130.69810.56250.067*
C350.8182 (6)0.6158 (6)0.7042 (4)0.0468 (13)
H350.70200.65710.69230.056*
C361.2771 (7)0.6114 (7)0.5565 (4)0.0684 (17)
H36A1.23270.62800.48760.082*
H36B1.31800.71860.57290.082*
C371.4299 (7)0.4809 (7)0.5443 (4)0.0622 (16)
H37A1.39020.37170.53110.075*
H37B1.48120.46900.61110.075*
N1S1.1372 (9)0.0804 (8)0.6005 (5)0.105 (2)
C1S1.0053 (11)0.0854 (8)0.6449 (6)0.077 (2)
C2S0.8316 (9)0.0914 (9)0.7021 (6)0.106 (2)
H2S10.75280.05350.65690.160*
H2S20.78910.20730.72380.160*
H2S30.83420.01740.76470.160*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Cu10.0282 (3)0.0198 (3)0.0365 (3)0.0045 (2)0.0048 (2)0.0014 (2)
O110.045 (2)0.0324 (18)0.044 (2)0.0143 (16)0.0101 (16)0.0085 (15)
O120.043 (2)0.0332 (19)0.045 (2)0.0158 (16)0.0044 (16)0.0070 (15)
O210.0339 (19)0.0395 (19)0.043 (2)0.0011 (15)0.0032 (15)0.0080 (15)
O220.0339 (19)0.0339 (18)0.0423 (19)0.0012 (15)0.0019 (15)0.0093 (15)
N310.031 (2)0.031 (2)0.036 (2)0.0069 (18)0.0005 (18)0.0012 (17)
C110.032 (3)0.023 (2)0.037 (3)0.001 (2)0.007 (2)0.000 (2)
C120.044 (3)0.027 (3)0.044 (3)0.010 (2)0.004 (2)0.004 (2)
C130.031 (3)0.020 (2)0.053 (3)0.001 (2)0.008 (2)0.005 (2)
C210.031 (3)0.019 (2)0.044 (3)0.008 (2)0.006 (2)0.003 (2)
C220.028 (3)0.023 (2)0.053 (3)0.006 (2)0.009 (2)0.003 (2)
C310.031 (3)0.031 (3)0.037 (3)0.004 (2)0.001 (2)0.004 (2)
C320.027 (3)0.039 (3)0.046 (3)0.001 (2)0.002 (2)0.001 (2)
C330.036 (3)0.036 (3)0.043 (3)0.006 (2)0.011 (2)0.001 (2)
C340.043 (3)0.071 (4)0.046 (3)0.001 (3)0.002 (3)0.020 (3)
C350.025 (3)0.062 (4)0.050 (3)0.002 (2)0.002 (2)0.014 (3)
C360.051 (4)0.074 (4)0.071 (4)0.010 (3)0.019 (3)0.015 (3)
C370.044 (3)0.076 (4)0.058 (4)0.008 (3)0.020 (3)0.001 (3)
N1S0.108 (5)0.103 (5)0.098 (5)0.003 (5)0.001 (4)0.017 (4)
C1S0.090 (6)0.062 (4)0.072 (5)0.008 (4)0.004 (4)0.004 (4)
C2S0.102 (6)0.084 (5)0.125 (6)0.007 (5)0.002 (5)0.003 (4)
Geometric parameters (Å, º) top
Cu1—O211.959 (3)C22—H22A0.9900
Cu1—O111.970 (3)C22—H22B0.9900
Cu1—O221.976 (3)C31—C321.364 (6)
Cu1—O121.994 (3)C31—H310.9500
Cu1—N312.163 (3)C32—C331.386 (6)
Cu1—Cu1i2.6392 (11)C32—H320.9500
O11—C111.271 (5)C33—C341.368 (6)
O12—C11i1.251 (5)C33—C361.526 (6)
O21—C211.263 (5)C34—C351.376 (6)
O22—C21i1.245 (5)C34—H340.9500
N31—C311.321 (5)C35—H350.9500
N31—C351.337 (5)C36—C371.470 (7)
C11—O12i1.251 (5)C36—H36A0.9900
C11—C121.510 (5)C36—H36B0.9900
C12—C131.525 (6)C37—C37iii1.508 (9)
C12—H12A0.9900C37—H37A0.9900
C12—H12B0.9900C37—H37B0.9900
C13—C22ii1.521 (5)N1S—C1S1.094 (8)
C13—H13A0.9900C1S—C2S1.435 (9)
C13—H13B0.9900C2S—H2S10.9800
C21—O22i1.245 (5)C2S—H2S20.9800
C21—C221.510 (5)C2S—H2S30.9800
C22—C13ii1.521 (5)
O21—Cu1—O1188.10 (13)C21—C22—C13ii111.1 (3)
O21—Cu1—O22167.84 (12)C21—C22—H22A109.4
O11—Cu1—O2290.17 (12)C13ii—C22—H22A109.4
O21—Cu1—O1291.43 (12)C21—C22—H22B109.4
O11—Cu1—O12168.18 (12)C13ii—C22—H22B109.4
O22—Cu1—O1287.80 (12)H22A—C22—H22B108.0
O21—Cu1—N3194.73 (13)N31—C31—C32124.2 (4)
O11—Cu1—N3197.41 (12)N31—C31—H31117.9
O22—Cu1—N3197.42 (13)C32—C31—H31117.9
O12—Cu1—N3194.39 (13)C31—C32—C33119.4 (4)
O21—Cu1—Cu1i82.35 (9)C31—C32—H32120.3
O11—Cu1—Cu1i84.67 (9)C33—C32—H32120.3
O22—Cu1—Cu1i85.51 (9)C34—C33—C32117.0 (4)
O12—Cu1—Cu1i83.57 (9)C34—C33—C36120.9 (4)
N31—Cu1—Cu1i176.38 (10)C32—C33—C36122.1 (5)
C11—O11—Cu1123.1 (3)C33—C34—C35119.8 (4)
C11i—O12—Cu1123.7 (3)C33—C34—H34120.1
C21—O21—Cu1125.6 (3)C35—C34—H34120.1
C21i—O22—Cu1121.4 (3)N31—C35—C34123.2 (4)
C31—N31—C35116.3 (4)N31—C35—H35118.4
C31—N31—Cu1121.7 (3)C34—C35—H35118.4
C35—N31—Cu1121.9 (3)C37—C36—C33117.4 (4)
O12i—C11—O11124.6 (4)C37—C36—H36A108.0
O12i—C11—C12118.6 (4)C33—C36—H36A108.0
O11—C11—C12116.8 (4)C37—C36—H36B108.0
C11—C12—C13115.4 (4)C33—C36—H36B108.0
C11—C12—H12A108.4H36A—C36—H36B107.2
C13—C12—H12A108.4C36—C37—C37iii113.3 (6)
C11—C12—H12B108.4C36—C37—H37A108.9
C13—C12—H12B108.4C37iii—C37—H37A108.9
H12A—C12—H12B107.5C36—C37—H37B108.9
C22ii—C13—C12112.7 (4)C37iii—C37—H37B108.9
C22ii—C13—H13A109.0H37A—C37—H37B107.7
C12—C13—H13A109.0N1S—C1S—C2S179.4 (10)
C22ii—C13—H13B109.0C1S—C2S—H2S1109.5
C12—C13—H13B109.0C1S—C2S—H2S2109.5
H13A—C13—H13B107.8H2S1—C2S—H2S2109.5
O22i—C21—O21124.9 (4)C1S—C2S—H2S3109.5
O22i—C21—C22117.9 (4)H2S1—C2S—H2S3109.5
O21—C21—C22117.1 (4)H2S2—C2S—H2S3109.5
Cu1—O11—C11—O12i7.5 (6)N31—C31—C32—C331.7 (7)
Cu1—O11—C11—C12170.5 (3)C31—C32—C33—C341.2 (7)
O12i—C11—C12—C1317.0 (6)C31—C32—C33—C36176.2 (4)
O11—C11—C12—C13164.8 (4)C32—C33—C34—C350.0 (7)
C11—C12—C13—C22ii175.8 (3)C36—C33—C34—C35177.4 (5)
Cu1—O21—C21—O22i5.5 (6)C31—N31—C35—C340.6 (7)
Cu1—O21—C21—C22171.3 (2)Cu1—N31—C35—C34176.5 (4)
O22i—C21—C22—C13ii91.8 (5)C33—C34—C35—N310.9 (8)
O21—C21—C22—C13ii85.2 (5)C34—C33—C36—C37147.8 (5)
C35—N31—C31—C320.7 (6)C32—C33—C36—C3734.8 (8)
Cu1—N31—C31—C32177.8 (3)C33—C36—C37—C37iii176.6 (5)
Symmetry codes: (i) x+1, y+1, z+2; (ii) x+1, y, z+2; (iii) x+3, y+1, z+1.
 

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