Buy article online - an online subscription or single-article purchase is required to access this article.
Download citation
Download citation
link to html
In the title compound, {[Pr(C12H15O6)(H2O)]·0.5H2O}n, the central praseodymium(III) cation is nine-coordinated by O atoms from six different chdc2− ligands (chdc2− is the 1,4-cyclo­hexane­dicarboxyl­ate dianion) and one terminal water mol­ecule. An inter­esting feature of the compound is the presence of two strands of cis-chdc2− ligands wrapped around each other, held together by praseodymium(III) cations to form a double-stranded chain. trans-Chdc2− ligands further bridge adjacent double-stranded chains to yield a three-dimensional framework.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806004491/rz6174sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536806004491/rz6174Isup2.hkl
Contains datablock I

CCDC reference: 601240

Key indicators

  • Single-crystal X-ray study
  • T = 292 K
  • Mean [sigma](C-C) = 0.008 Å
  • H-atom completeness 84%
  • Disorder in solvent or counterion
  • R factor = 0.036
  • wR factor = 0.085
  • Data-to-parameter ratio = 17.1

checkCIF/PLATON results

No syntax errors found



Alert level C PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings Differ .... ? PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT045_ALERT_1_C Calculated and Reported Z Differ by ............ 0.50 Ratio PLAT302_ALERT_4_C Anion/Solvent Disorder ......................... 50.00 Perc. PLAT764_ALERT_4_C Overcomplete CIF Bond List Detected (Rep/Expd) . 1.33 Ratio
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:C12 H18 O7.5 Pr1 Atom count from the _atom_site data: C12 H15 O7.5 Pr1 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 2 From the CIF: _chemical_formula_sum C12 H18 O7.5 Pr TEST: Compare cell contents of formula and atom_site data atom Z*formula cif sites diff C 24.00 24.00 0.00 H 36.00 30.00 6.00 O 15.00 15.00 0.00 Pr 2.00 2.00 0.00
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 5 ALERT level C = Check and explain 3 ALERT level G = General alerts; check 5 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 1 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 2 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: PROCESS-AUTO (Rigaku, 1998); cell refinement: PROCESS-AUTO; data reduction: PROCESS-AUTO; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL-Plus (Sheldrick, 1990).

poly[[aqua(µ4-1,4-cyclohexanedicarboxylato)praseodymium(III)] hemihydrate] top
Crystal data top
[Pr(C12H15O6)(H2O)]·0.5H2OZ = 2
Mr = 423.18F(000) = 412
Triclinic, P1Dx = 1.966 Mg m3
Hall symbol: -p 1Melting point: not measured K
a = 7.9451 (16) ÅMo Kα radiation, λ = 0.71073 Å
b = 9.0421 (18) ÅCell parameters from 7113 reflections
c = 10.538 (2) Åθ = 3.2–27.5°
α = 72.22 (3)°µ = 3.44 mm1
β = 84.09 (3)°T = 292 K
γ = 84.01 (3)°Block, green
V = 714.9 (3) Å30.37 × 0.33 × 0.24 mm
Data collection top
Rigaku R-AXIS RAPID
diffractometer
3257 independent reflections
Radiation source: rotor target2757 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.046
Detector resolution: 10.0 pixels mm-1θmax = 27.5°, θmin = 3.2°
ω scansh = 910
Absorption correction: multi-scan
(ABSCOR; Higashi, 1995)
k = 1111
Tmin = 0.313, Tmax = 0.438l = 1313
7113 measured reflections
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)] = 0.036Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.085H-atom parameters constrained
S = 1.11 w = 1/[σ2(Fo2) + (0.041P)2]
where P = (Fo2 + 2Fc2)/3
3257 reflections(Δ/σ)max < 0.001
191 parametersΔρmax = 0.78 e Å3
1 restraintΔρmin = 0.78 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)
C10.0612 (7)0.0401 (6)0.2534 (5)0.0211 (11)
C20.0140 (8)0.0124 (7)0.1376 (5)0.0239 (12)
H20.13040.01640.16640.029*
C30.0205 (9)0.1559 (7)0.0177 (6)0.0355 (15)
H3A0.09240.19210.00710.043*
H3B0.09370.23790.04110.043*
C40.0869 (9)0.1235 (7)0.1021 (6)0.0341 (15)
H4A0.08090.21590.17870.041*
H4B0.20500.10090.08140.041*
C50.4567 (6)0.3221 (6)0.7366 (5)0.0194 (11)
H50.47880.25830.82770.023*
C60.5901 (7)0.4400 (6)0.6932 (6)0.0219 (11)
H6A0.70160.38590.68900.026*
H6B0.57010.50900.60460.026*
C70.5854 (7)0.5351 (6)0.7898 (6)0.0225 (11)
H7A0.66770.61280.75720.027*
H7B0.61720.46730.87610.027*
C100.2717 (7)0.5010 (6)0.8431 (6)0.0242 (12)
H8A0.28540.43140.93250.029*
H8B0.16070.55700.84330.029*
C80.4079 (7)0.6171 (6)0.8068 (5)0.0214 (11)
H90.40870.65810.88280.026*
C110.2807 (7)0.4052 (6)0.7456 (6)0.0238 (12)
H10A0.25470.47320.65790.029*
H10B0.19670.32890.77510.029*
C120.4678 (7)0.2115 (6)0.6533 (5)0.0180 (11)
C90.3691 (7)0.7549 (6)0.6866 (6)0.0204 (11)
O10.0075 (4)0.0361 (4)0.3730 (4)0.0200 (8)
O20.1766 (5)0.1289 (5)0.2350 (4)0.0277 (9)
O30.3334 (5)0.1828 (5)0.6143 (4)0.0299 (10)
O40.6133 (5)0.1504 (5)0.6283 (4)0.0296 (9)
O50.2246 (5)0.7814 (5)0.6450 (5)0.0332 (10)
O60.4831 (5)0.8512 (4)0.6328 (4)0.0238 (8)
O1W0.0731 (5)0.3089 (5)0.4242 (5)0.0334 (10)
O2W0.4967 (12)0.1018 (12)0.0775 (10)0.047 (3)0.50
Pr10.25493 (3)0.04192 (3)0.47339 (3)0.01486 (10)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
C10.021 (3)0.026 (3)0.017 (3)0.001 (2)0.000 (2)0.008 (2)
C20.032 (3)0.031 (3)0.012 (3)0.005 (2)0.003 (2)0.009 (2)
C30.053 (4)0.029 (3)0.027 (3)0.003 (3)0.012 (3)0.011 (3)
C40.046 (4)0.029 (3)0.028 (3)0.004 (3)0.020 (3)0.007 (3)
C50.020 (2)0.020 (3)0.021 (3)0.003 (2)0.001 (2)0.010 (2)
C60.021 (3)0.023 (3)0.023 (3)0.002 (2)0.000 (2)0.009 (2)
C70.028 (3)0.018 (3)0.024 (3)0.000 (2)0.011 (2)0.006 (2)
C100.029 (3)0.019 (3)0.024 (3)0.004 (2)0.009 (2)0.008 (2)
C80.032 (3)0.017 (3)0.019 (3)0.003 (2)0.004 (2)0.009 (2)
C110.022 (3)0.019 (3)0.034 (3)0.006 (2)0.001 (2)0.012 (2)
C120.027 (3)0.016 (2)0.015 (3)0.003 (2)0.004 (2)0.008 (2)
C90.022 (3)0.015 (3)0.023 (3)0.001 (2)0.002 (2)0.005 (2)
O10.0149 (17)0.033 (2)0.0158 (19)0.0042 (15)0.0024 (15)0.0112 (17)
O20.025 (2)0.040 (2)0.020 (2)0.0126 (18)0.0012 (17)0.0103 (19)
O30.025 (2)0.041 (3)0.035 (2)0.0038 (18)0.0014 (18)0.028 (2)
O40.024 (2)0.033 (2)0.040 (3)0.0043 (17)0.0077 (19)0.024 (2)
O50.0194 (19)0.027 (2)0.046 (3)0.0035 (16)0.0044 (19)0.002 (2)
O60.0249 (19)0.0189 (19)0.026 (2)0.0073 (15)0.0010 (17)0.0023 (17)
O1W0.031 (2)0.025 (2)0.042 (3)0.0010 (17)0.007 (2)0.006 (2)
O2W0.059 (6)0.046 (6)0.039 (6)0.019 (5)0.023 (5)0.021 (5)
Pr10.01306 (14)0.01581 (14)0.01755 (15)0.00114 (9)0.00284 (10)0.00712 (11)
Geometric parameters (Å, º) top
C1—O21.243 (6)C8—C91.512 (8)
C1—O11.290 (7)C8—H90.9800
C1—C21.509 (7)C11—H10A0.9700
C2—C31.510 (8)C11—H10B0.9700
C2—C41.518 (9)C12—O31.261 (6)
C2—H20.9800C12—O41.266 (7)
C3—C4i1.534 (8)C9—O51.245 (7)
C3—H3A0.9700C9—O61.288 (6)
C3—H3B0.9700C9—Pr1ii2.996 (6)
C4—C3i1.534 (8)O1—Pr1iii2.500 (4)
C4—H4A0.9700O1—Pr12.580 (3)
C4—H4B0.9700O2—Pr12.516 (4)
C5—C121.510 (6)O3—Pr12.393 (4)
C5—C61.519 (7)O4—Pr1iv2.408 (4)
C5—C111.525 (7)O5—Pr1ii2.511 (4)
C5—H50.9800O6—Pr1v2.408 (4)
C6—C71.516 (7)O6—Pr1ii2.699 (4)
C6—H6A0.9700O1W—Pr12.616 (4)
C6—H6B0.9700Pr1—O4iv2.408 (4)
C7—C81.544 (8)Pr1—O6v2.408 (4)
C7—H7A0.9700Pr1—O1iii2.500 (4)
C7—H7B0.9700Pr1—O5vi2.511 (4)
C10—C111.525 (7)Pr1—O6vi2.699 (4)
C10—C81.525 (7)Pr1—C9vi2.996 (6)
C10—H8A0.9700Pr1—Pr1iv3.9532 (11)
C10—H8B0.9700
O2—C1—O1120.5 (5)C1—O1—Pr1iii138.5 (3)
O2—C1—C2121.3 (5)C1—O1—Pr191.6 (3)
O1—C1—C2118.2 (5)Pr1iii—O1—Pr1109.51 (13)
C1—C2—C3112.3 (5)C1—O2—Pr195.8 (3)
C1—C2—C4109.1 (5)C12—O3—Pr1137.7 (4)
C3—C2—C4111.1 (5)C12—O4—Pr1iv140.3 (3)
C1—C2—H2108.1C9—O5—Pr1ii100.3 (3)
C3—C2—H2108.1C9—O6—Pr1v162.2 (4)
C4—C2—H2108.1C9—O6—Pr1ii90.2 (3)
C2—C3—C4i111.8 (5)Pr1v—O6—Pr1ii101.28 (14)
C2—C3—H3A109.3O3—Pr1—O4iv137.42 (13)
C4i—C3—H3A109.3O3—Pr1—O6v75.37 (14)
C2—C3—H3B109.3O4iv—Pr1—O6v76.49 (14)
C4i—C3—H3B109.3O3—Pr1—O1iii78.93 (12)
H3A—C3—H3B107.9O4iv—Pr1—O1iii130.31 (13)
C2—C4—C3i112.1 (5)O6v—Pr1—O1iii152.55 (12)
C2—C4—H4A109.2O3—Pr1—O5vi98.96 (15)
C3i—C4—H4A109.2O4iv—Pr1—O5vi73.44 (16)
C2—C4—H4B109.2O6v—Pr1—O5vi126.36 (13)
C3i—C4—H4B109.2O1iii—Pr1—O5vi67.05 (14)
H4A—C4—H4B107.9O3—Pr1—O2131.96 (15)
C12—C5—C6113.6 (5)O4iv—Pr1—O273.22 (14)
C12—C5—C11113.2 (4)O6v—Pr1—O281.39 (13)
C6—C5—C11110.1 (4)O1iii—Pr1—O2109.65 (12)
C12—C5—H5106.5O5vi—Pr1—O2128.40 (14)
C6—C5—H5106.5O3—Pr1—O1145.73 (13)
C11—C5—H5106.5O4iv—Pr1—O176.23 (12)
C7—C6—C5111.1 (5)O6v—Pr1—O1130.23 (12)
C7—C6—H6A109.4O1iii—Pr1—O170.49 (13)
C5—C6—H6A109.4O5vi—Pr1—O183.31 (13)
C7—C6—H6B109.4O2—Pr1—O151.11 (12)
C5—C6—H6B109.4O3—Pr1—O1W71.29 (14)
H6A—C6—H6B108.0O4iv—Pr1—O1W143.14 (15)
C6—C7—C8111.9 (4)O6v—Pr1—O1W95.81 (14)
C6—C7—H7A109.2O1iii—Pr1—O1W66.56 (14)
C8—C7—H7A109.2O5vi—Pr1—O1W133.60 (14)
C6—C7—H7B109.2O2—Pr1—O1W69.98 (14)
C8—C7—H7B109.2O1—Pr1—O1W82.42 (12)
H7A—C7—H7B107.9O3—Pr1—O6vi73.70 (13)
C11—C10—C8112.1 (4)O4iv—Pr1—O6vi69.92 (13)
C11—C10—H8A109.2O6v—Pr1—O6vi78.72 (14)
C8—C10—H8A109.2O1iii—Pr1—O6vi103.21 (12)
C11—C10—H8B109.2O5vi—Pr1—O6vi49.57 (12)
C8—C10—H8B109.2O2—Pr1—O6vi141.20 (13)
H8A—C10—H8B107.9O1—Pr1—O6vi127.57 (12)
C9—C8—C10112.6 (5)O1W—Pr1—O6vi144.80 (13)
C9—C8—C7112.3 (5)O3—Pr1—C9vi85.78 (15)
C10—C8—C7110.9 (4)O4iv—Pr1—C9vi70.54 (15)
C9—C8—H9106.9O6v—Pr1—C9vi103.47 (14)
C10—C8—H9106.9O1iii—Pr1—C9vi83.92 (14)
C7—C8—H9106.9O5vi—Pr1—C9vi24.13 (13)
C10—C11—C5110.9 (4)O2—Pr1—C9vi140.97 (14)
C10—C11—H10A109.5O1—Pr1—C9vi105.48 (13)
C5—C11—H10A109.5O1W—Pr1—C9vi145.19 (15)
C10—C11—H10B109.5O6vi—Pr1—C9vi25.46 (12)
C5—C11—H10B109.5O3—Pr1—Pr1iv69.79 (10)
H10A—C11—H10B108.1O4iv—Pr1—Pr1iv67.87 (9)
O3—C12—O4123.6 (4)O6v—Pr1—Pr1iv42.04 (9)
O3—C12—C5119.0 (5)O1iii—Pr1—Pr1iv134.16 (8)
O4—C12—C5117.4 (4)O5vi—Pr1—Pr1iv85.31 (9)
O5—C9—O6119.8 (5)O2—Pr1—Pr1iv116.16 (9)
O5—C9—C8120.5 (5)O1—Pr1—Pr1iv144.07 (8)
O6—C9—C8119.6 (5)O1W—Pr1—Pr1iv128.29 (9)
O5—C9—Pr1ii55.6 (3)O6vi—Pr1—Pr1iv36.68 (8)
O6—C9—Pr1ii64.3 (3)C9vi—Pr1—Pr1iv61.66 (10)
C8—C9—Pr1ii172.1 (4)
Symmetry codes: (i) x, y, z; (ii) x, y+1, z; (iii) x, y, z+1; (iv) x+1, y, z+1; (v) x+1, y+1, z+1; (vi) x, y1, z.
 

Subscribe to Acta Crystallographica Section E: Crystallographic Communications

The full text of this article is available to subscribers to the journal.

If you have already registered and are using a computer listed in your registration details, please email support@iucr.org for assistance.

Buy online

You may purchase this article in PDF and/or HTML formats. For purchasers in the European Community who do not have a VAT number, VAT will be added at the local rate. Payments to the IUCr are handled by WorldPay, who will accept payment by credit card in several currencies. To purchase the article, please complete the form below (fields marked * are required), and then click on `Continue'.
E-mail address* 
Repeat e-mail address* 
(for error checking) 

Format*   PDF (US $40)
   HTML (US $40)
   PDF+HTML (US $50)
In order for VAT to be shown for your country javascript needs to be enabled.

VAT number 
(non-UK EC countries only) 
Country* 
 

Terms and conditions of use
Contact us

Follow Acta Cryst. E
Sign up for e-alerts
Follow Acta Cryst. on Twitter
Follow us on facebook
Sign up for RSS feeds