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The title complex, [Rh(C8H12)(C9H16N2O2)(H2O)](BF4) or [RhL(COD)(H2O)](BF4), is a monomer in the solid state. The RhI centre is in a square-planar arrangement. The four coordination sites are occupied by the N atom of the pyrazole ligand, the O atom from a water mol­ecule and the centroids of the two cyclo­octa­diene olefin bonds. The structure is stabilized by hydrogen bonds between the coordinated water mol­ecule and the two O atoms of the ether groups of the pyrazole ligand and one of the F atoms of the BF4 unit.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536803016155/tk6126sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536803016155/tk6126Isup2.hkl
Contains datablock I

CCDC reference: 221652

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](C-C) = 0.007 Å
  • R factor = 0.043
  • wR factor = 0.117
  • Data-to-parameter ratio = 15.7

checkCIF results

No syntax errors found

ADDSYM reports no extra symmetry








Computing details top

Data collection: IPDS (Stoe & Cie, 2000); cell refinement: IPDS; data reduction: X-RED (Stoe & Cie, 1996); program(s) used to solve structure: SIR92 (Altomare et al., 1993); 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).

Aqua(η4–1,5-cyclooctadiene)[1-(2-methoxyethoxymethyl)- 3,5-dimethylpyrazole]rhodium(I) tetrafluoroborate top
Crystal data top
[Rh(C8H12)(C9H16N2O2)(H2O)](BF4)F(000) = 1024
Mr = 500.15Dx = 1.575 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybcCell parameters from 8000 reflections
a = 10.0023 (10) Åθ = 2.1–26.1°
b = 23.2203 (17) ŵ = 0.86 mm1
c = 9.2977 (10) ÅT = 293 K
β = 102.368 (12)°Block, yellow
V = 2109.3 (4) Å30.30 × 0.25 × 0.20 mm
Z = 4
Data collection top
Stoe IPDS
diffractometer
3630 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.027
φ scansθmax = 26.1°, θmin = 2.1°
Absorption correction: part of the refinement model (ΔF)
(Parkin, S. et al. 1995)
h = 1212
Tmin = 0.776, Tmax = 0.837k = 2827
16245 measured reflectionsl = 1111
4070 independent 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)] = 0.043Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.117H atoms treated by a mixture of independent and constrained refinement
S = 0.99 w = 1/[σ2(Fo2) + (0.0689P)2 + 4.0982P]
where P = (Fo2 + 2Fc2)/3
4070 reflections(Δ/σ)max < 0.001
260 parametersΔρmax = 0.90 e Å3
3 restraintsΔρmin = 0.68 e Å3
Special details top

Experimental. The data were collected on a Stoe Imaging Plate Diffraction System (IPDS). The crystal-to-detector distance was 70 mm. 152 frames (2 min per frame) were obtained with 0 < φ < 198.9° and with the crystals rotated through 1.3° in φ. Coverage of the unique set was over 97% complete to at least 26.09°.

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
C30.0431 (4)0.1707 (2)0.1141 (6)0.0594 (12)
C40.0172 (4)0.1408 (2)0.2292 (5)0.0616 (12)
H40.06920.14100.32490.074*
C50.1032 (4)0.1091 (2)0.1772 (4)0.0499 (10)
C60.1589 (6)0.2102 (3)0.1058 (9)0.094 (2)
H6A0.14740.22500.00750.113*
H6B0.24360.18940.13110.113*
H6C0.16020.24150.17340.113*
C70.1757 (6)0.0699 (2)0.2573 (5)0.0679 (14)
H7A0.25570.05520.19150.082*
H7B0.20230.09020.33660.082*
H7C0.11650.03840.29630.082*
C80.0912 (5)0.1849 (2)0.1467 (5)0.0594 (11)
H8A0.01460.20830.16020.071*
H8B0.10680.15560.22280.071*
C110.1891 (6)0.2665 (2)0.0585 (7)0.0746 (15)
H11A0.12120.29320.07920.090*
H11B0.15850.25220.04120.090*
C120.3220 (7)0.2952 (3)0.0745 (10)0.097 (2)
H12A0.31340.32880.01120.117*
H12B0.35460.30760.17560.117*
C140.5276 (8)0.2804 (4)0.0027 (13)0.144 (4)
H14A0.49810.30870.07800.172*
H14B0.58020.25130.03860.172*
H14C0.58290.29850.08240.172*
C210.3261 (4)0.0217 (3)0.4232 (5)0.0667 (14)
H21A0.35490.01800.44190.080*
H21B0.34120.04140.51740.080*
C220.4144 (4)0.04942 (18)0.3301 (4)0.0439 (8)
H220.47740.07870.38180.053*
C230.4621 (4)0.02082 (16)0.2209 (4)0.0425 (8)
H230.55250.03370.20940.051*
C240.4301 (5)0.0406 (2)0.1751 (6)0.0628 (12)
H24A0.47320.04950.09370.075*
H24B0.47030.06570.25650.075*
C250.2823 (5)0.0536 (2)0.1302 (7)0.0743 (16)
H25A0.25430.07380.21020.089*
H25B0.26820.07950.04630.089*
C260.1906 (4)0.00171 (19)0.0897 (5)0.0499 (9)
H260.12640.00490.00570.060*
C270.1430 (4)0.03170 (18)0.1930 (4)0.0449 (8)
H270.05160.04790.15590.054*
C280.1763 (5)0.0226 (3)0.3556 (5)0.0625 (12)
H28A0.13650.01360.37720.075*
H28B0.13380.05310.40160.075*
B10.7996 (5)0.1222 (2)0.3265 (6)0.0491 (10)
F10.9197 (3)0.14890 (16)0.3789 (4)0.0886 (10)
F20.8175 (6)0.0704 (2)0.2741 (9)0.184 (3)
F30.7379 (5)0.1170 (3)0.4425 (6)0.147 (2)
F40.7116 (4)0.15416 (18)0.2259 (5)0.1083 (13)
N10.0571 (3)0.15740 (15)0.0043 (4)0.0493 (8)
N20.1488 (3)0.11937 (15)0.0341 (3)0.0427 (7)
O100.2070 (4)0.21926 (15)0.1620 (4)0.0634 (8)
O130.4149 (4)0.25550 (17)0.0350 (6)0.0979 (15)
O10.4428 (3)0.14028 (12)0.0913 (4)0.0526 (7)
Rh10.29942 (3)0.076409 (12)0.12152 (3)0.03547 (13)
H1b0.524 (2)0.1385 (16)0.142 (4)0.043*
H1a0.423 (4)0.1759 (9)0.081 (4)0.043*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
C30.043 (2)0.064 (3)0.071 (3)0.0082 (19)0.011 (2)0.031 (2)
C40.048 (2)0.081 (3)0.050 (2)0.009 (2)0.0034 (18)0.030 (2)
C50.047 (2)0.069 (3)0.0341 (18)0.0075 (19)0.0080 (15)0.0081 (17)
C60.056 (3)0.080 (4)0.144 (6)0.022 (3)0.017 (3)0.042 (4)
C70.074 (3)0.096 (4)0.038 (2)0.014 (3)0.020 (2)0.016 (2)
C80.072 (3)0.060 (3)0.055 (2)0.020 (2)0.033 (2)0.001 (2)
C110.077 (3)0.046 (3)0.105 (4)0.018 (2)0.030 (3)0.005 (3)
C120.086 (4)0.055 (3)0.150 (6)0.013 (3)0.023 (4)0.001 (4)
C140.082 (5)0.104 (6)0.261 (12)0.013 (4)0.072 (6)0.075 (7)
C210.049 (2)0.113 (4)0.036 (2)0.007 (2)0.0037 (17)0.005 (2)
C220.0390 (18)0.047 (2)0.0397 (18)0.0049 (15)0.0039 (15)0.0018 (16)
C230.0363 (17)0.041 (2)0.047 (2)0.0071 (15)0.0035 (15)0.0015 (15)
C240.070 (3)0.044 (2)0.070 (3)0.011 (2)0.004 (2)0.009 (2)
C250.061 (3)0.045 (3)0.117 (5)0.007 (2)0.019 (3)0.018 (3)
C260.0410 (19)0.054 (2)0.053 (2)0.0102 (17)0.0059 (16)0.0100 (18)
C270.0359 (17)0.057 (2)0.0408 (19)0.0022 (16)0.0052 (14)0.0031 (17)
C280.053 (2)0.090 (4)0.044 (2)0.004 (2)0.0077 (18)0.016 (2)
B10.039 (2)0.042 (2)0.065 (3)0.0039 (18)0.009 (2)0.007 (2)
F10.0619 (18)0.093 (2)0.104 (2)0.0247 (16)0.0036 (16)0.0014 (19)
F20.131 (4)0.119 (4)0.274 (8)0.040 (3)0.017 (4)0.121 (5)
F30.097 (3)0.220 (6)0.136 (4)0.002 (3)0.050 (3)0.063 (4)
F40.096 (3)0.103 (3)0.104 (3)0.004 (2)0.027 (2)0.019 (2)
N10.0473 (17)0.055 (2)0.0494 (18)0.0155 (15)0.0181 (15)0.0114 (15)
N20.0411 (16)0.056 (2)0.0326 (14)0.0106 (14)0.0120 (12)0.0043 (13)
O100.076 (2)0.0573 (19)0.0597 (19)0.0116 (16)0.0209 (16)0.0103 (15)
O130.081 (3)0.056 (2)0.171 (5)0.0175 (19)0.058 (3)0.035 (3)
O10.0449 (15)0.0381 (15)0.074 (2)0.0022 (12)0.0114 (14)0.0076 (13)
Rh10.03480 (18)0.03818 (19)0.03272 (18)0.00378 (10)0.00567 (12)0.00176 (10)
Geometric parameters (Å, º) top
Rh1—O12.123 (3)C14—H14A0.9600
Rh1—N22.103 (3)C14—H14B0.9600
Rh1—C222.126 (4)C14—H14C0.9600
Rh1—C232.127 (3)C21—C281.496 (6)
Rh1—C262.104 (4)C21—C221.507 (6)
Rh1—C272.101 (4)C21—H21A0.9700
C3—C41.347 (7)C21—H21B0.9700
C3—N11.356 (5)C22—C231.381 (5)
C3—C61.491 (7)C22—H220.9800
C4—C51.405 (6)C23—C241.504 (6)
C4—H40.9300C23—H230.9800
C5—N21.332 (5)C24—C251.479 (7)
C5—C71.464 (7)C24—H24A0.9700
C6—H6A0.9600C24—H24B0.9700
C6—H6B0.9600C25—C261.512 (7)
C6—H6C0.9600C25—H25A0.9700
C7—H7A0.9600C25—H25B0.9700
C7—H7B0.9600C26—C271.396 (6)
C7—H7C0.9600C26—H260.9800
C8—O101.388 (6)C27—C281.492 (5)
C8—N11.443 (6)C27—H270.9800
C8—H8A0.9700C28—H28A0.9700
C8—H8B0.9700C28—H28B0.9700
C11—O101.444 (7)B1—F21.324 (6)
C11—C121.467 (8)B1—F11.347 (5)
C11—H11A0.9700B1—F31.358 (6)
C11—H11B0.9700B1—F41.359 (6)
C12—O131.412 (7)N1—N21.374 (4)
C12—H12A0.9700O1—H1b0.845 (18)
C12—H12B0.9700O1—H1a0.852 (18)
C14—O131.377 (7)
O1—Rh1—N288.99 (12)H12A—C12—H12B108.4
O1—Rh1—C2294.45 (14)O13—C14—H14A109.5
O1—Rh1—C2390.33 (13)O13—C14—H14B109.5
O1—Rh1—C26158.08 (15)O13—C14—H14C109.5
O1—Rh1—C27163.13 (14)H14A—C14—H14B109.5
N2—Rh1—C22159.22 (13)H14A—C14—H14C109.5
N2—Rh1—C23162.80 (13)H14B—C14—H14C109.5
N2—Rh1—C2692.26 (15)C28—C21—C22114.2 (4)
N2—Rh1—C2788.83 (14)C28—C21—H21A108.7
C22—Rh1—C2337.89 (15)C22—C21—H21A108.7
C22—Rh1—C2692.09 (16)C28—C21—H21B108.7
C22—Rh1—C2781.95 (15)C22—C21—H21B108.7
C23—Rh1—C2682.09 (16)H21A—C21—H21B107.6
C23—Rh1—C2796.61 (15)C23—C22—C21123.7 (4)
C26—Rh1—C2738.77 (16)C23—C22—H22114.1
Rh1—N2—N1123.1 (2)C21—C22—H22114.1
Rh1—N2—C5130.1 (3)Rh1—C22—H22114.1
Rh1—C22—C21112.4 (3)C22—C23—C24125.3 (4)
Rh1—C22—C2371.1 (2)C22—C23—H23113.9
Rh1—C23—C2271.0 (2)C24—C23—H23113.9
Rh1—C23—C24110.9 (3)Rh1—C23—H23113.9
Rh1—C26—C25112.6 (3)C25—C24—C23114.3 (4)
Rh1—C26—C2770.5 (2)C25—C24—H24A108.7
Rh1—C27—C2670.7 (2)C23—C24—H24A108.7
Rh1—C27—C28111.7 (3)C25—C24—H24B108.7
C4—C3—N1107.0 (4)C23—C24—H24B108.7
C4—C3—C6129.9 (5)H24A—C24—H24B107.6
N1—C3—C6123.0 (5)C24—C25—C26115.1 (4)
C3—C4—C5107.1 (4)C24—C25—H25A108.5
C3—C4—H4126.5C26—C25—H25A108.5
C5—C4—H4126.5C24—C25—H25B108.5
N2—C5—C4109.6 (4)C26—C25—H25B108.5
N2—C5—C7121.2 (4)H25A—C25—H25B107.5
C4—C5—C7129.2 (4)C27—C26—C25123.4 (4)
C3—C6—H6A109.5C27—C26—H26114.2
C3—C6—H6B109.5C25—C26—H26114.2
H6A—C6—H6B109.5Rh1—C26—H26114.2
C3—C6—H6C109.5C26—C27—C28125.7 (4)
H6A—C6—H6C109.5C26—C27—H27113.6
H6B—C6—H6C109.5C28—C27—H27113.6
C5—C7—H7A109.5Rh1—C27—H27113.6
C5—C7—H7B109.5C27—C28—C21114.5 (4)
H7A—C7—H7B109.5C27—C28—H28A108.6
C5—C7—H7C109.5C21—C28—H28A108.6
H7A—C7—H7C109.5C27—C28—H28B108.6
H7B—C7—H7C109.5C21—C28—H28B108.6
O10—C8—N1112.1 (3)H28A—C28—H28B107.6
O10—C8—H8A109.2F2—B1—F1111.8 (4)
N1—C8—H8A109.2F2—B1—F3109.4 (6)
O10—C8—H8B109.2F1—B1—F3105.9 (5)
N1—C8—H8B109.2F2—B1—F4111.2 (5)
H8A—C8—H8B107.9F1—B1—F4113.2 (4)
O10—C11—C12107.3 (5)F3—B1—F4104.9 (4)
O10—C11—H11A110.3C3—N1—N2110.7 (4)
C12—C11—H11A110.3C3—N1—C8129.2 (4)
O10—C11—H11B110.3N2—N1—C8118.8 (3)
C12—C11—H11B110.3C5—N2—N1105.6 (3)
H11A—C11—H11B108.5C8—O10—C11112.7 (4)
O13—C12—C11108.0 (5)C14—O13—C12114.4 (6)
O13—C12—H12A110.1Rh1—O1—H1b119 (3)
C11—C12—H12A110.1Rh1—O1—H1a123 (3)
O13—C12—H12B110.1H1b—O1—H1a106 (3)
C11—C12—H12B110.1
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1—H1a···O100.85 (2)2.64 (3)3.166 (4)121 (3)
O1—H1a···O130.85 (2)1.89 (2)2.729 (5)167 (4)
O1—H1b···F40.85 (2)1.91 (2)2.731 (5)164 (4)
 

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