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The title compound is a binuclear lanthanum(III) complex having each metal ion in deca­coordination with oxygen atoms from 1,4-chdc2− ligands, acetate groups and coordinated water mol­ecules to form a distorted bicapped square anti­prismatic geometry. The strong inter­molecular O–H...O and weak C–H...O inter­actions lead to the construction of a three-dimensional supra­molecular architecture.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S2056989017016103/vn2132sup1.cif
Contains datablock I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2056989017016103/vn2132Isup2.hkl
Contains datablock I

CCDC reference: 1546730

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](C-C) = 0.016 Å
  • R factor = 0.041
  • wR factor = 0.146
  • Data-to-parameter ratio = 13.8

checkCIF/PLATON results

No syntax errors found



Alert level C PLAT342_ALERT_3_C Low Bond Precision on C-C Bonds ............... 0.01589 Ang.
Alert level G PLAT002_ALERT_2_G Number of Distance or Angle Restraints on AtSite 9 Note 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 PLAT083_ALERT_2_G SHELXL Second Parameter in WGHT Unusually Large 6.15 Why ? PLAT154_ALERT_1_G The s.u.'s on the Cell Angles are Equal ..(Note) 0.005 Degree PLAT171_ALERT_4_G The CIF-Embedded .res File Contains EADP Records 3 Report PLAT172_ALERT_4_G The CIF-Embedded .res File Contains DFIX Records 6 Report PLAT180_ALERT_4_G Check Cell Rounding: # of Values Ending with 0 = 3 Note PLAT199_ALERT_1_G Reported _cell_measurement_temperature ..... (K) 293 Check PLAT200_ALERT_1_G Reported _diffrn_ambient_temperature ..... (K) 293 Check PLAT764_ALERT_4_G Overcomplete CIF Bond List Detected (Rep/Expd) . 1.36 Ratio PLAT790_ALERT_4_G Centre of Gravity not Within Unit Cell: Resd. # 2 Note H2 O PLAT860_ALERT_3_G Number of Least-Squares Restraints ............. 9 Note PLAT870_ALERT_4_G ALERTS Related to Twinning Effects Suppressed .. ! Info PLAT910_ALERT_3_G Missing # of FCF Reflection(s) Below Theta(Min). 1 Note
0 ALERT level A = Most likely a serious problem - resolve or explain 0 ALERT level B = A potentially serious problem, consider carefully 1 ALERT level C = Check. Ensure it is not caused by an omission or oversight 16 ALERT level G = General information/check it is not something unexpected 5 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 2 ALERT type 2 Indicator that the structure model may be wrong or deficient 3 ALERT type 3 Indicator that the structure quality may be low 6 ALERT type 4 Improvement, methodology, query or suggestion 1 ALERT type 5 Informative message, check

Computing details top

Data collection: APEX2 (Bruker, 2004); cell refinement: APEX2 and SAINT (Bruker, 2004); data reduction: SAINT and XPREP (Bruker, 2004); program(s) used to solve structure: SIR92 (Sheldrick, 2015); program(s) used to refine structure: SHELXL2014 (Sheldrick, 2015); molecular graphics: DIAMOND (Brandenburg, 2010); software used to prepare material for publication: SHELXL2014 (Sheldrick, 2015) and publCIF (Westrip, 2010)'.

Poly[[di-µ3-acetato-tetraaquabis(µ2-cyclohexane-1,4-dicarboxylato)dilanthanum(III)] dihydrate] top
Crystal data top
[La2(C2H3O2)2(C8H10O4)2(H2O)4]·2H2OZ = 1
Mr = 844.32F(000) = 416
Triclinic, P1Dx = 1.960 Mg m3
a = 6.9341 (8) ÅMo Kα radiation, λ = 0.71073 Å
b = 8.9597 (13) ÅCell parameters from 7100 reflections
c = 12.3030 (16) Åθ = 2.8–30.9°
α = 110.217 (5)°µ = 3.02 mm1
β = 91.060 (5)°T = 293 K
γ = 93.280 (5)°Block, colourless
V = 715.49 (16) Å30.20 × 0.15 × 0.15 mm
Data collection top
Bruker Kappa APEXII CCD
diffractometer
2815 independent reflections
Radiation source: Sealed tube2447 reflections with I > 2σ(I)
ω and φ scanθmax = 26.0°, θmin = 2.4°
Absorption correction: multi-scan
(SADABS; Bruker, 2004)
h = 88
Tmin = 0.60, Tmax = 0.74k = 1110
2818 measured reflectionsl = 015
Refinement top
Refinement on F29 restraints
Least-squares matrix: fullHydrogen site location: mixed
R[F2 > 2σ(F2)] = 0.041H atoms treated by a mixture of independent and constrained refinement
wR(F2) = 0.146 w = 1/[σ2(Fo2) + (0.0821P)2 + 6.1459P]
where P = (Fo2 + 2Fc2)/3
S = 1.07(Δ/σ)max = 0.005
2818 reflectionsΔρmax = 2.17 e Å3
204 parametersΔρmin = 2.46 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.

Refinement. Refined as a two-component twin.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
C10.2377 (17)0.7936 (10)0.7752 (7)0.0203 (18)
C20.2486 (18)0.7706 (11)0.8920 (8)0.030 (2)
H20.24470.87600.95220.036*
C30.0724 (17)0.6681 (16)0.9058 (11)0.033 (3)
H3A0.06980.67150.98550.040*
H3B0.04480.71160.88890.040*
C40.0778 (17)0.4962 (14)0.8253 (10)0.030 (3)
H4A0.06940.49190.74550.036*
H4B0.03310.43390.83790.036*
C50.2631 (16)0.4239 (11)0.8460 (7)0.024 (2)
H50.26330.41960.92450.028*
C60.4375 (16)0.5264 (15)0.8372 (11)0.030 (3)
H6A0.44680.52130.75740.036*
H6B0.55260.48360.85760.036*
C70.4325 (17)0.6994 (14)0.9147 (10)0.028 (2)
H7A0.54380.76020.90100.034*
H7B0.44030.70670.99520.034*
C80.2736 (16)0.2574 (10)0.7614 (8)0.0229 (19)
C90.7522 (14)1.0347 (9)0.6555 (7)0.0141 (16)
C100.7542 (18)1.0729 (13)0.7831 (8)0.030 (2)
H10A0.70301.17490.81940.046*
H10B0.88461.07580.81180.046*
H10C0.67630.99260.80060.046*
O10.3916 (11)0.7991 (10)0.7225 (7)0.0280 (18)
O20.0804 (11)0.8116 (10)0.7334 (7)0.0272 (18)
O30.0144 (11)0.6946 (10)0.4871 (7)0.0310 (18)
O40.3865 (13)0.6914 (10)0.4470 (8)0.039 (2)
O50.5999 (10)0.9978 (10)0.5957 (6)0.0219 (16)
O60.9100 (10)1.0455 (9)0.6066 (6)0.0220 (16)
O70.2827 (11)0.2366 (7)0.6530 (5)0.0223 (14)
O80.2635 (12)0.1397 (7)0.7932 (5)0.0283 (15)
O90.2682 (13)0.6345 (9)0.6499 (7)0.0384 (18)
La10.23952 (8)0.92768 (5)0.58722 (4)0.01486 (18)
H4C0.474 (15)0.704 (14)0.398 (8)0.05 (3)*
H4D0.326 (16)0.597 (8)0.406 (8)0.05 (3)*
H3C0.088 (14)0.668 (17)0.538 (9)0.06 (3)*
H3D0.105 (12)0.705 (17)0.437 (9)0.06 (3)*
H9A0.207 (15)0.687 (15)0.719 (6)0.06 (3)*
H9B0.388 (9)0.669 (17)0.663 (10)0.06 (3)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
C10.026 (5)0.012 (4)0.025 (4)0.004 (4)0.006 (5)0.008 (3)
C20.047 (7)0.023 (5)0.019 (4)0.003 (5)0.002 (5)0.008 (4)
C30.029 (7)0.041 (7)0.034 (7)0.011 (5)0.007 (5)0.017 (6)
C40.031 (7)0.027 (6)0.030 (6)0.004 (5)0.003 (4)0.005 (5)
C50.030 (6)0.026 (5)0.016 (4)0.005 (4)0.002 (4)0.011 (4)
C60.022 (6)0.037 (7)0.033 (6)0.004 (5)0.005 (4)0.014 (5)
C70.041 (8)0.025 (6)0.017 (5)0.001 (5)0.004 (4)0.007 (4)
C80.017 (5)0.024 (5)0.029 (5)0.002 (4)0.001 (4)0.012 (4)
C90.010 (4)0.012 (3)0.018 (4)0.003 (4)0.002 (4)0.001 (3)
C100.026 (6)0.042 (6)0.020 (4)0.006 (5)0.003 (5)0.007 (4)
O10.016 (4)0.039 (5)0.039 (5)0.005 (3)0.005 (3)0.025 (4)
O20.026 (5)0.031 (5)0.028 (4)0.004 (3)0.005 (3)0.015 (4)
O30.026 (5)0.035 (5)0.034 (5)0.005 (3)0.002 (3)0.017 (4)
O40.033 (5)0.022 (4)0.051 (5)0.009 (3)0.023 (4)0.001 (4)
O50.012 (4)0.037 (4)0.020 (4)0.001 (3)0.002 (3)0.014 (3)
O60.011 (4)0.032 (4)0.025 (4)0.001 (3)0.002 (3)0.011 (3)
O70.025 (4)0.024 (3)0.018 (3)0.001 (3)0.006 (3)0.007 (2)
O80.042 (4)0.021 (3)0.024 (3)0.001 (4)0.004 (3)0.011 (3)
O90.023 (5)0.033 (4)0.057 (5)0.004 (4)0.004 (4)0.013 (4)
La10.0121 (3)0.0169 (3)0.0169 (3)0.0017 (2)0.0015 (2)0.00745 (18)
Geometric parameters (Å, º) top
C1—O21.240 (13)C9—La1ii3.119 (8)
C1—O11.266 (13)C10—H10A0.9600
C1—C21.522 (12)C10—H10B0.9600
C1—La12.952 (8)C10—H10C0.9600
C2—C71.521 (17)O1—La12.570 (7)
C2—C31.533 (17)O2—La12.601 (8)
C2—H20.9800O3—La12.588 (8)
C3—C41.519 (18)O3—H3C0.90 (2)
C3—H3A0.9700O3—H3D0.90 (2)
C3—H3B0.9700O4—La12.506 (8)
C4—C51.527 (16)O4—H4C0.90 (2)
C4—H4A0.9700O4—H4D0.89 (2)
C4—H4B0.9700O5—La12.533 (7)
C5—C81.502 (12)O5—La1ii2.792 (7)
C5—C61.505 (15)O6—La1iii2.552 (7)
C5—H50.9800O6—La1ii2.674 (7)
C6—C71.516 (17)O7—La1i2.598 (6)
C6—H6A0.9700O8—La1i2.585 (6)
C6—H6B0.9700O9—H9A0.90 (2)
C7—H7A0.9700O9—H9B0.90 (2)
C7—H7B0.9700La1—O6iv2.552 (7)
C8—O81.244 (11)La1—O8v2.585 (6)
C8—O71.284 (11)La1—O7v2.598 (6)
C8—La1i2.983 (9)La1—O6ii2.674 (7)
C9—O51.237 (11)La1—O5ii2.792 (7)
C9—O61.273 (11)La1—C8v2.983 (9)
C9—C101.487 (11)
O2—C1—O1120.1 (8)C9—O6—La1ii98.1 (5)
O2—C1—C2120.4 (9)La1iii—O6—La1ii115.2 (3)
O1—C1—C2119.5 (10)C8—O7—La1i94.3 (5)
O2—C1—La161.6 (5)C8—O8—La1i96.0 (5)
O1—C1—La160.2 (5)H9A—O9—H9B101 (3)
C2—C1—La1164.8 (6)O4—La1—O573.2 (3)
C1—C2—C7114.2 (9)O4—La1—O6iv135.8 (3)
C1—C2—C3110.9 (9)O5—La1—O6iv143.4 (2)
C7—C2—C3109.4 (8)O4—La1—O177.7 (3)
C1—C2—H2107.4O5—La1—O173.8 (2)
C7—C2—H2107.4O6iv—La1—O1126.4 (2)
C3—C2—H2107.4O4—La1—O8v146.0 (3)
C4—C3—C2111.4 (9)O5—La1—O8v82.5 (3)
C4—C3—H3A109.4O6iv—La1—O8v76.9 (2)
C2—C3—H3A109.4O1—La1—O8v72.8 (2)
C4—C3—H3B109.4O4—La1—O367.5 (3)
C2—C3—H3B109.4O5—La1—O3140.7 (3)
H3A—C3—H3B108.0O6iv—La1—O373.0 (3)
C3—C4—C5111.4 (10)O1—La1—O396.1 (3)
C3—C4—H4A109.4O8v—La1—O3131.7 (3)
C5—C4—H4A109.4O4—La1—O7v138.0 (2)
C3—C4—H4B109.4O5—La1—O7v73.7 (2)
C5—C4—H4B109.4O6iv—La1—O7v69.9 (2)
H4A—C4—H4B108.0O1—La1—O7v116.4 (2)
C8—C5—C6110.0 (9)O8v—La1—O7v49.88 (18)
C8—C5—C4111.2 (9)O3—La1—O7v140.6 (2)
C6—C5—C4110.4 (8)O4—La1—O2103.1 (3)
C8—C5—H5108.4O5—La1—O2121.8 (2)
C6—C5—H5108.4O6iv—La1—O278.8 (2)
C4—C5—H5108.4O1—La1—O249.7 (2)
C5—C6—C7113.4 (9)O8v—La1—O269.9 (2)
C5—C6—H6A108.9O3—La1—O267.7 (3)
C7—C6—H6A108.9O7v—La1—O2116.2 (2)
C5—C6—H6B108.9O4—La1—O6ii83.0 (3)
C7—C6—H6B108.9O5—La1—O6ii107.7 (2)
H6A—C6—H6B107.7O6iv—La1—O6ii64.8 (3)
C6—C7—C2111.4 (9)O1—La1—O6ii159.3 (3)
C6—C7—H7A109.3O8v—La1—O6ii127.8 (2)
C2—C7—H7A109.3O3—La1—O6ii69.3 (2)
C6—C7—H7B109.3O7v—La1—O6ii83.2 (2)
C2—C7—H7B109.3O2—La1—O6ii129.9 (2)
H7A—C7—H7B108.0O4—La1—O5ii68.8 (3)
O8—C8—O7119.6 (8)O5—La1—O5ii61.3 (3)
O8—C8—C5121.6 (8)O6iv—La1—O5ii103.7 (2)
O7—C8—C5118.7 (7)O1—La1—O5ii129.6 (2)
O8—C8—La1i59.5 (5)O8v—La1—O5ii119.3 (2)
O7—C8—La1i60.3 (4)O3—La1—O5ii104.2 (2)
C5—C8—La1i172.5 (8)O7v—La1—O5ii72.9 (2)
O5—C9—O6118.9 (7)O2—La1—O5ii170.7 (2)
O5—C9—C10121.7 (9)O6ii—La1—O5ii46.51 (19)
O6—C9—C10119.4 (9)O4—La1—C193.6 (3)
O5—C9—La1ii63.3 (4)O5—La1—C197.2 (3)
O6—C9—La1ii58.1 (4)O6iv—La1—C1101.4 (3)
C10—C9—La1ii161.8 (6)O1—La1—C125.3 (3)
C9—C10—H10A109.5O8v—La1—C165.9 (2)
C9—C10—H10B109.5O3—La1—C184.1 (3)
H10A—C10—H10B109.5O7v—La1—C1115.7 (2)
C9—C10—H10C109.5O2—La1—C124.8 (3)
H10A—C10—H10C109.5O6ii—La1—C1152.5 (3)
H10B—C10—H10C109.5O5ii—La1—C1154.8 (3)
C1—O1—La194.4 (6)O4—La1—C8v151.3 (3)
C1—O2—La193.6 (6)O5—La1—C8v78.0 (3)
La1—O3—H3C113 (9)O6iv—La1—C8v70.6 (3)
La1—O3—H3D120 (9)O1—La1—C8v94.8 (3)
H3C—O3—H3D101 (3)O8v—La1—C8v24.5 (2)
La1—O4—H4C121 (8)O3—La1—C8v141.2 (3)
La1—O4—H4D127 (8)O7v—La1—C8v25.4 (2)
H4C—O4—H4D102 (3)O2—La1—C8v92.3 (3)
C9—O5—La1147.1 (6)O6ii—La1—C8v105.7 (2)
C9—O5—La1ii93.4 (5)O5ii—La1—C8v97.0 (2)
La1—O5—La1ii118.7 (3)C1—La1—C8v90.4 (2)
C9—O6—La1iii138.0 (6)
O2—C1—C2—C7161.8 (9)C4—C5—C8—O763.7 (13)
O1—C1—C2—C720.4 (13)O2—C1—O1—La115.4 (9)
La1—C1—C2—C7105 (3)C2—C1—O1—La1162.5 (7)
O2—C1—C2—C337.7 (12)O1—C1—O2—La115.2 (9)
O1—C1—C2—C3144.5 (9)C2—C1—O2—La1162.6 (7)
La1—C1—C2—C3131 (3)O6—C9—O5—La1174.3 (8)
C1—C2—C3—C469.6 (12)C10—C9—O5—La18.2 (16)
C7—C2—C3—C457.2 (11)La1ii—C9—O5—La1168.1 (12)
C2—C3—C4—C557.2 (12)O6—C9—O5—La1ii17.7 (8)
C3—C4—C5—C8176.5 (9)C10—C9—O5—La1ii159.9 (7)
C3—C4—C5—C654.1 (12)O5—C9—O6—La1iii124.4 (8)
C8—C5—C6—C7176.5 (9)C10—C9—O6—La1iii58.0 (12)
C4—C5—C6—C753.4 (11)La1ii—C9—O6—La1iii143.1 (9)
C5—C6—C7—C255.0 (12)O5—C9—O6—La1ii18.6 (9)
C1—C2—C7—C669.6 (12)C10—C9—O6—La1ii158.9 (7)
C3—C2—C7—C655.3 (11)O8—C8—O7—La1i4.7 (11)
C6—C5—C8—O8124.8 (11)C5—C8—O7—La1i171.5 (9)
C4—C5—C8—O8112.5 (12)O7—C8—O8—La1i4.8 (11)
C6—C5—C8—O759.0 (13)C5—C8—O8—La1i171.4 (9)
Symmetry codes: (i) x, y1, z; (ii) x+1, y+2, z+1; (iii) x+1, y, z; (iv) x1, y, z; (v) x, y+1, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
C10—H10C···O10.962.493.295 (14)141
O4—H4C···O7vi0.90 (2)1.92 (5)2.771 (10)158 (12)
O4—H4D···O9vii0.89 (2)1.96 (6)2.812 (11)158 (12)
O3—H3C···O90.90 (2)1.97 (3)2.858 (12)172 (13)
O3—H3D···O7vii0.90 (2)1.86 (3)2.750 (11)170 (14)
O9—H9A···O20.90 (2)2.20 (11)2.786 (12)122 (11)
O9—H9B···O1iv0.90 (2)1.97 (5)2.846 (11)164 (13)
Symmetry codes: (iv) x1, y, z; (vi) x+1, y+1, z+1; (vii) x, y+1, z+1.
 

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