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The title compound, [Pr(C5HF6O2)3(C6H14O3)] or [Pr(hfpd)3(2g)], was prepared by the reaction of PrCl3·7H2O and hfpd-H (1,1,1,5,5,5-hexafluoro­pentane-2,4-dione) in the presence of aqueous ammonia and recrystallization of the product from n-hexane in the presence of diglyme (2g). The metal atom is nine-coordinate, bonded to three bidentate β-di­ketonato ligands and the polyether mol­ecule.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536803016556/dn6077sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536803016556/dn6077Isup2.hkl
Contains datablock I

CCDC reference: 225648

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](C-C) = 0.003 Å
  • R factor = 0.035
  • wR factor = 0.086
  • Data-to-parameter ratio = 8.6

checkCIF/PLATON results

No syntax errors found



Alert level A PLAT027_ALERT_3_A _diffrn_reflns_theta_full too Low .............. 24.94 Deg. PLAT029_ALERT_3_A _diffrn_measured_fraction_theta_full Low ....... 0.82 PLAT242_ALERT_2_A Check Low U(eq) as Compared to Neighbors .... C15
Author Response: This alarm is due to the high ADPs of all fluorine atoms in the six CF3 groups. In particular, four (out of six) -CF~3~ groups of the compound were disordered between two orientations and were assigned partial occupancy.

Alert level B REFLT03_ALERT_3_B Reflection count < 90% complete (theta max?) From the CIF: _diffrn_reflns_theta_max 24.94 From the CIF: _diffrn_reflns_theta_full 0.00 From the CIF: _reflns_number_total 4785 TEST2: Reflns within _diffrn_reflns_theta_max Count of symmetry unique reflns 5629 Completeness (_total/calc) 85.01% PLAT022_ALERT_3_B Ratio Unique / Expected Reflections too Low .... 0.85
Author Response: Same as above.
PLAT242_ALERT_2_B Check Low    U(eq) as Compared to Neighbors ....         C1
Author Response: This alarm is due to the high ADPs of all fluorine atoms in the six CF3 groups. In particular, four (out of six) -CF~3~ groups of the compound were disordered between two orientations and were assigned partial occupancy.
PLAT242_ALERT_2_B Check Low    U(eq) as Compared to Neighbors ....         C5
Author Response: This alarm is due to the high ADPs of all fluorine atoms in the six CF3 groups. In particular, four (out of six) -CF~3~ groups of the compound were disordered between two orientations and were assigned partial occupancy.
PLAT242_ALERT_2_B Check Low    U(eq) as Compared to Neighbors ....         C6
Author Response: This alarm is due to the high ADPs of all fluorine atoms in the six CF3 groups. In particular, four (out of six) -CF~3~ groups of the compound were disordered between two orientations and were assigned partial occupancy.
PLAT242_ALERT_2_B Check Low    U(eq) as Compared to Neighbors ....        C10
Author Response: This alarm is due to the high ADPs of all fluorine atoms in the six CF3 groups. In particular, four (out of six) -CF~3~ groups of the compound were disordered between two orientations and were assigned partial occupancy.
PLAT242_ALERT_2_B Check Low    U(eq) as Compared to Neighbors ....        C11
Author Response: This alarm is due to the high ADPs of all fluorine atoms in the six CF3 groups. In particular, four (out of six) -CF~3~ groups of the compound were disordered between two orientations and were assigned partial occupancy.

Alert level C REFNR01_ALERT_3_C Ratio of reflections to parameters is < 10 for a centrosymmetric structure sine(theta)/lambda -0.2695 Proportion of unique data used 1.0000 Ratio reflections to parameters 8.6216 PLAT062_ALERT_4_C Rescale T(min) & T(max) by ..................... 0.97 PLAT088_ALERT_3_C Poor Data / Parameter Ratio .................... 8.62
Author Response: This is an inevitable consequence of the introduction of additional parameters to treat the disordered F atoms.
PLAT213_ALERT_2_C Atom F2B     has ADP max/min Ratio .............       3.70 prolat
Author Response: The high ADP max/min ratio for the F atoms is attributed to disorder. In particular, four (out of six) -CF~3~ groups of the compound were disordered between two orientations and were assigned partial occupancy.
PLAT242_ALERT_2_C Check Low    U(eq) as Compared to Neighbors ....         C2
Author Response: This alarm is due to the high ADPs of all fluorine atoms in the six CF3 groups. In particular, four (out of six) -CF~3~ groups of the compound were disordered between two orientations and were assigned partial occupancy.
PLAT242_ALERT_2_C Check Low    U(eq) as Compared to Neighbors ....         C7
Author Response: This alarm is due to the high ADPs of all fluorine atoms in the six CF3 groups. In particular, four (out of six) -CF~3~ groups of the compound were disordered between two orientations and were assigned partial occupancy.
PLAT301_ALERT_3_C Main Residue  Disorder .........................      20.00 Perc.
PLAT779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ......      39.50 Deg.
              F1A  -C1   -F1B     1.555   1.555   1.555
PLAT779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ......      43.20 Deg.
              F2B  -C1   -F2A     1.555   1.555   1.555
PLAT779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ......      37.50 Deg.
              F12B -C10  -F12A    1.555   1.555   1.555
PLAT779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ......      43.20 Deg.
              F11A -C10  -F11B    1.555   1.555   1.555
PLAT779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ......      43.10 Deg.
              F15B -C11  -F15A    1.555   1.555   1.555
PLAT779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ......      41.90 Deg.
              F14B -C11  -F14A    1.555   1.555   1.555
PLAT779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ......      42.90 Deg.
              F13A -C11  -F13B    1.555   1.555   1.555

3 ALERT level A = In general: serious problem 7 ALERT level B = Potentially serious problem 14 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 16 ALERT type 2 Indicator that the structure model may be wrong or deficient 7 ALERT type 3 Indicator that the structure quality may be low 1 ALERT type 4 Improvement, methodology, query or suggestion

Computing details top

Data collection: Mar Research image-plate scanner software; cell refinement: XDS (Kabsch, 1993); data reduction: XDS; program(s) used to solve structure: SIR97 (Altomare et al., 1999) and SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 (Farrugia, 1997); software used to prepare material for publication: SHELXL97.

(I) top
Crystal data top
[Pr(C6H14O3)(C5HF6O2)3]F(000) = 1744
Mr = 896.26Dx = 1.848 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybcCell parameters from 4409 reflections
a = 10.013 (3) Åθ = 2.5–24.0°
b = 15.656 (4) ŵ = 1.66 mm1
c = 21.133 (5) ÅT = 293 K
β = 103.48 (4)°Prism, green
V = 3221.7 (15) Å30.45 × 0.30 × 0.20 mm
Z = 4
Data collection top
Mar Research Image Plate Scanner
diffractometer
4785 independent reflections
Radiation source: fine-focus sealed tube4219 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.039
rotation method scansθmax = 24.9°, θmin = 2.5°
Absorption correction: empirical (using intensity measurements)
(XDS; Kabsch, 1993)
h = 1111
Tmin = 0.542, Tmax = 0.741k = 018
9202 measured reflectionsl = 2424
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.035H-atom parameters constrained
wR(F2) = 0.086 w = 1/[σ2(Fo2) + (0.0312P)2 + 8.0994P]
where P = (Fo2 + 2Fc2)/3
S = 1.09(Δ/σ)max = 0.010
4785 reflectionsΔρmax = 0.84 e Å3
555 parametersΔρmin = 0.71 e Å3
228 restraintsExtinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.00417 (8)
Special details top

Experimental. Each crystal was mounted on a Mar Research Image Plate Scanner and 95 frames were measured with an exposure time of 120 s per frame. Scan mode: omega/2theta. The crystal-detector distance was 75 mm. Data were processed using the XDS package.

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)
Pr10.069057 (10)0.188557 (7)0.375402 (5)0.04224 (3)
O10.13948 (15)0.12542 (10)0.30245 (7)0.0603 (5)
O20.08399 (14)0.18612 (10)0.26125 (7)0.0563 (4)
O30.07670 (15)0.30667 (9)0.32247 (7)0.0571 (4)
O40.10505 (14)0.21586 (9)0.43552 (7)0.0525 (4)
O50.14084 (15)0.32476 (9)0.43135 (7)0.0578 (5)
O60.22596 (14)0.16472 (8)0.48402 (7)0.0509 (4)
O70.30949 (14)0.23393 (10)0.35791 (7)0.0618 (5)
O80.23969 (15)0.06558 (9)0.36708 (7)0.0581 (4)
O90.01139 (15)0.03882 (9)0.41508 (8)0.0631 (5)
C20.1872 (2)0.11907 (14)0.24269 (10)0.0556 (6)
C30.1233 (2)0.13855 (17)0.19336 (11)0.0655 (8)
H30.17030.13060.15030.079*
C40.0094 (2)0.16973 (14)0.20684 (10)0.0524 (6)
C70.1727 (2)0.34812 (13)0.33597 (11)0.0560 (7)
C80.2325 (2)0.33367 (15)0.38621 (12)0.0649 (8)
H80.30310.37040.39020.078*
C90.1991 (2)0.27019 (13)0.43169 (10)0.0511 (6)
C120.2285 (2)0.34887 (13)0.47987 (10)0.0517 (6)
C130.3135 (2)0.29909 (13)0.52667 (11)0.0540 (6)
H130.37720.32530.56010.065*
C140.3050 (2)0.21078 (13)0.52447 (10)0.0482 (6)
C160.3199 (3)0.31355 (17)0.32600 (15)0.0888 (10)
H16A0.26970.35670.34300.133*
H16B0.28230.30740.28010.133*
H16C0.41460.33000.33350.133*
C170.3851 (2)0.16765 (17)0.33431 (12)0.0708 (8)
H17A0.47970.18530.33860.085*
H17B0.34490.15660.28870.085*
C180.3801 (2)0.08940 (17)0.37303 (13)0.0709 (8)
H18A0.42900.04350.35740.085*
H18B0.42390.09990.41840.085*
C190.2275 (3)0.01017 (15)0.40322 (13)0.0754 (9)
H19A0.26760.00090.44910.090*
H19B0.27580.05700.38830.090*
C200.0799 (3)0.03094 (14)0.39315 (13)0.0833 (10)
H20A0.04060.04140.34730.100*
H20B0.06870.08220.41720.100*
C210.1245 (3)0.01409 (17)0.41996 (13)0.0842 (9)
H21A0.16860.06150.43550.126*
H21B0.11810.03280.44980.126*
H21C0.17730.00290.37790.126*
C10.3335 (3)0.08497 (17)0.22402 (12)0.0893 (10)
F1A0.3732 (3)0.0455 (2)0.16808 (15)0.1251 (12)0.513 (2)
F2A0.4167 (3)0.1525 (3)0.22269 (19)0.1410 (16)0.513 (2)
F3A0.3691 (3)0.0337 (3)0.26662 (18)0.1528 (14)0.513 (2)
F1B0.3936 (3)0.1010 (3)0.16187 (15)0.1162 (14)0.487 (2)
F2B0.4124 (3)0.1134 (3)0.25827 (17)0.1455 (15)0.487 (2)
F3B0.3242 (4)0.0009 (3)0.2344 (2)0.1479 (17)0.487 (2)
C50.0765 (3)0.18856 (18)0.14975 (12)0.0715 (8)
F40.20657 (16)0.16964 (15)0.16407 (8)0.1161 (8)
F50.0204 (2)0.14662 (16)0.09587 (8)0.1253 (8)
F60.0668 (2)0.26896 (12)0.13475 (9)0.1318 (7)
C60.22559 (18)0.42011 (13)0.28763 (10)0.1005 (12)
F7A0.1827 (8)0.4903 (3)0.3201 (3)0.158 (3)0.175 (2)
F8A0.3601 (4)0.4133 (6)0.2697 (4)0.150 (3)0.175 (2)
F9A0.1777 (6)0.4129 (6)0.23526 (19)0.147 (3)0.175 (2)
F7B0.3146 (2)0.47148 (14)0.30611 (13)0.1539 (10)0.825 (2)
F8B0.2858 (3)0.38816 (18)0.23078 (10)0.1648 (13)0.825 (2)
F9B0.1263 (3)0.46869 (13)0.27741 (13)0.1432 (10)0.825 (2)
C100.2833 (2)0.25884 (15)0.48230 (11)0.0704 (8)
F10A0.3045 (4)0.3319 (2)0.51236 (15)0.1082 (11)0.5178 (18)
F11A0.3997 (3)0.2229 (3)0.45974 (17)0.1325 (14)0.5178 (18)
F12A0.2226 (3)0.2120 (2)0.53337 (14)0.0956 (10)0.5178 (18)
F10B0.3939 (3)0.3058 (3)0.47125 (19)0.1170 (14)0.4822 (18)
F11B0.3333 (3)0.1790 (2)0.47713 (19)0.1109 (13)0.4822 (18)
F12B0.2152 (4)0.2643 (3)0.53961 (16)0.1280 (16)0.4822 (18)
C110.2446 (2)0.44698 (15)0.48712 (11)0.0755 (9)
F13A0.2482 (3)0.48447 (19)0.43297 (16)0.1293 (15)0.514 (2)
F14A0.3568 (3)0.4718 (2)0.52958 (17)0.1234 (15)0.514 (2)
F15A0.1377 (4)0.4794 (2)0.50489 (14)0.1262 (14)0.514 (2)
F13B0.3396 (3)0.4702 (2)0.45603 (19)0.1300 (15)0.486 (2)
F14B0.2791 (4)0.4712 (2)0.54695 (14)0.1229 (15)0.486 (2)
F15B0.1322 (4)0.4863 (2)0.45923 (17)0.1459 (18)0.486 (2)
C150.4018 (3)0.16205 (16)0.57834 (12)0.0655 (8)
F160.51845 (18)0.20016 (13)0.60288 (10)0.1298 (8)
F170.3473 (2)0.14388 (14)0.62608 (8)0.1299 (7)
F180.4370 (2)0.08789 (12)0.55864 (10)0.1590 (8)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Pr10.04514 (5)0.04373 (5)0.03962 (5)0.00202 (4)0.01347 (5)0.00231 (4)
O10.0584 (8)0.0752 (9)0.0485 (7)0.0124 (7)0.0153 (7)0.0008 (7)
O20.0532 (7)0.0735 (9)0.0446 (7)0.0017 (7)0.0162 (6)0.0013 (6)
O30.0653 (8)0.0578 (8)0.0495 (7)0.0097 (7)0.0157 (7)0.0097 (6)
O40.0537 (7)0.0562 (7)0.0519 (7)0.0058 (6)0.0208 (6)0.0059 (6)
O50.0666 (8)0.0475 (7)0.0575 (8)0.0063 (6)0.0107 (7)0.0004 (6)
O60.0535 (7)0.0465 (7)0.0490 (7)0.0020 (6)0.0043 (7)0.0009 (6)
O70.0571 (7)0.0719 (9)0.0617 (8)0.0058 (7)0.0244 (7)0.0019 (7)
O80.0622 (8)0.0553 (8)0.0569 (8)0.0135 (7)0.0142 (7)0.0060 (6)
O90.0673 (8)0.0497 (7)0.0715 (9)0.0046 (7)0.0143 (8)0.0110 (7)
C20.0479 (10)0.0658 (12)0.0538 (11)0.0005 (10)0.0131 (10)0.0045 (10)
C30.0586 (12)0.0934 (16)0.0445 (11)0.0007 (12)0.0120 (11)0.0040 (11)
C40.0536 (10)0.0613 (12)0.0452 (10)0.0111 (9)0.0173 (9)0.0066 (9)
C70.0611 (12)0.0481 (10)0.0553 (12)0.0015 (10)0.0062 (11)0.0075 (9)
C80.0535 (12)0.0710 (14)0.0660 (14)0.0041 (11)0.0053 (12)0.0143 (11)
C90.0458 (10)0.0562 (11)0.0520 (11)0.0044 (9)0.0131 (9)0.0098 (9)
C120.0616 (10)0.0458 (10)0.0548 (11)0.0026 (9)0.0279 (9)0.0071 (8)
C130.0548 (11)0.0529 (11)0.0525 (11)0.0061 (9)0.0087 (10)0.0084 (9)
C140.0462 (10)0.0567 (11)0.0429 (10)0.0017 (9)0.0132 (9)0.0020 (8)
C160.0954 (16)0.0830 (17)0.0968 (19)0.0261 (14)0.0400 (14)0.0064 (14)
C170.0437 (10)0.1028 (18)0.0700 (14)0.0002 (11)0.0218 (10)0.0162 (13)
C180.0551 (11)0.0847 (15)0.0735 (15)0.0185 (11)0.0162 (11)0.0067 (12)
C190.0947 (16)0.0477 (11)0.0824 (16)0.0175 (12)0.0178 (14)0.0015 (11)
C200.131 (2)0.0356 (11)0.0804 (16)0.0079 (13)0.0197 (16)0.0078 (11)
C210.0786 (15)0.0817 (15)0.0901 (17)0.0238 (13)0.0154 (14)0.0277 (13)
C10.0645 (14)0.116 (2)0.0850 (18)0.0199 (15)0.0124 (14)0.0202 (16)
F1A0.0956 (18)0.191 (3)0.0911 (18)0.0702 (18)0.0269 (16)0.0764 (17)
F2A0.0764 (16)0.241 (4)0.120 (3)0.006 (2)0.0517 (17)0.007 (3)
F3A0.1082 (18)0.232 (3)0.117 (2)0.1030 (18)0.0238 (18)0.021 (2)
F1B0.0677 (18)0.194 (3)0.075 (2)0.041 (2)0.0093 (17)0.001 (2)
F2B0.0737 (14)0.274 (4)0.114 (2)0.049 (2)0.0727 (14)0.078 (2)
F3B0.129 (2)0.170 (3)0.144 (3)0.084 (2)0.032 (2)0.029 (3)
C50.0645 (13)0.1029 (18)0.0480 (12)0.0027 (13)0.0148 (11)0.0096 (12)
F40.0752 (8)0.209 (2)0.0736 (9)0.0257 (11)0.0369 (8)0.0277 (11)
F50.1299 (12)0.1939 (19)0.0642 (9)0.0312 (13)0.0472 (9)0.0284 (11)
F60.1822 (16)0.1083 (12)0.1277 (12)0.0137 (12)0.0821 (11)0.0540 (9)
C60.120 (2)0.0730 (16)0.102 (2)0.0349 (15)0.0121 (19)0.0240 (15)
F7A0.197 (6)0.096 (5)0.181 (6)0.033 (5)0.048 (5)0.067 (5)
F8A0.176 (6)0.138 (5)0.127 (5)0.072 (5)0.012 (5)0.054 (5)
F9A0.201 (6)0.117 (5)0.115 (5)0.020 (5)0.018 (5)0.082 (4)
F7B0.1808 (17)0.1188 (13)0.171 (2)0.0982 (12)0.0603 (16)0.0646 (13)
F8B0.215 (3)0.156 (2)0.0849 (13)0.019 (2)0.0426 (17)0.0387 (14)
F9B0.178 (2)0.0852 (12)0.1711 (18)0.0047 (14)0.0507 (16)0.0703 (11)
C100.0593 (11)0.0851 (16)0.0758 (14)0.0027 (11)0.0342 (10)0.0028 (12)
F10A0.161 (2)0.0919 (19)0.0932 (18)0.0151 (18)0.0724 (17)0.0173 (15)
F11A0.0605 (14)0.239 (3)0.100 (2)0.0748 (18)0.0219 (15)0.033 (2)
F12A0.0988 (16)0.1085 (19)0.0974 (17)0.0337 (15)0.0591 (14)0.0459 (14)
F10B0.0790 (15)0.164 (3)0.129 (2)0.0311 (18)0.0674 (15)0.007 (2)
F11B0.0826 (17)0.145 (3)0.119 (2)0.0285 (18)0.0520 (16)0.015 (2)
F12B0.114 (2)0.209 (4)0.0667 (18)0.030 (3)0.0311 (19)0.043 (2)
C110.0943 (17)0.0506 (12)0.0808 (16)0.0046 (12)0.0188 (14)0.0053 (12)
F13A0.233 (3)0.0517 (15)0.109 (2)0.010 (2)0.051 (2)0.0191 (15)
F14A0.126 (2)0.0607 (16)0.161 (3)0.0278 (17)0.012 (2)0.0174 (19)
F15A0.157 (2)0.0668 (17)0.172 (3)0.0231 (18)0.074 (2)0.0243 (18)
F13B0.173 (3)0.0711 (19)0.158 (3)0.0423 (19)0.063 (2)0.013 (2)
F14B0.219 (4)0.0640 (17)0.0878 (19)0.015 (2)0.039 (2)0.0365 (15)
F15B0.167 (3)0.0576 (18)0.191 (4)0.035 (2)0.004 (3)0.012 (2)
C150.0635 (13)0.0750 (14)0.0537 (12)0.0010 (12)0.0049 (12)0.0077 (11)
F160.0808 (11)0.1421 (14)0.1335 (14)0.0282 (10)0.0420 (11)0.0533 (11)
F170.1129 (12)0.1845 (16)0.0950 (10)0.0283 (12)0.0300 (10)0.0784 (10)
F180.1773 (15)0.1196 (12)0.1318 (15)0.0932 (10)0.0619 (13)0.0226 (11)
Geometric parameters (Å, º) top
Pr1—O42.4225 (17)C17—H17B0.9700
Pr1—O22.4517 (16)C18—H18A0.9700
Pr1—O32.4576 (15)C18—H18B0.9700
Pr1—O52.4629 (15)C19—C201.480 (4)
Pr1—O62.4891 (17)C19—H19A0.9700
Pr1—O12.4927 (17)C19—H19B0.9700
Pr1—O92.5995 (16)C20—H20A0.9700
Pr1—O82.6072 (15)C20—H20B0.9700
Pr1—O72.6176 (17)C21—H21A0.9600
O1—C21.246 (3)C21—H21B0.9600
O2—C41.243 (2)C21—H21C0.9600
O3—C71.247 (3)C1—F2B1.270 (4)
O4—C91.258 (2)C1—F1A1.311 (4)
O5—C121.243 (2)C1—F3A1.316 (5)
O6—C141.250 (2)C1—F3B1.334 (5)
O7—C161.433 (3)C1—F1B1.335 (4)
O7—C171.441 (3)C1—F2A1.342 (5)
O8—C191.431 (3)C5—F61.296 (3)
O8—C181.432 (3)C5—F41.301 (3)
O9—C201.424 (3)C5—F51.321 (3)
O9—C211.441 (3)C6—F9B1.309 (3)
C2—C31.378 (3)C6—F9A1.310 (5)
C2—C11.522 (3)C6—F8B1.311 (3)
C3—C41.382 (3)C6—F7A1.315 (5)
C3—H30.9300C6—F8A1.316 (4)
C4—C51.540 (4)C6—F7B1.325 (3)
C7—C81.354 (4)C10—F12B1.247 (4)
C7—C61.530 (3)C10—F11A1.282 (4)
C8—C91.369 (3)C10—F10B1.305 (4)
C8—H80.9300C10—F12A1.329 (4)
C9—C101.518 (3)C10—F11B1.342 (4)
C12—C131.385 (3)C10—F10A1.349 (4)
C12—C111.548 (3)C11—F14B1.288 (4)
C13—C141.385 (3)C11—F13A1.294 (4)
C13—H130.9300C11—F15B1.298 (4)
C14—C151.518 (3)C11—F15A1.316 (4)
C16—H16A0.9600C11—F14A1.322 (4)
C16—H16B0.9600C11—F13B1.326 (5)
C16—H16C0.9600C15—F171.286 (3)
C17—C181.481 (4)C15—F161.306 (3)
C17—H17A0.9700C15—F181.309 (3)
O4—Pr1—O2137.32 (5)O9—C20—H20B109.9
O4—Pr1—O371.48 (5)C19—C20—H20B109.9
O2—Pr1—O374.32 (5)H20A—C20—H20B108.3
O4—Pr1—O576.15 (5)O9—C21—H21A109.5
O2—Pr1—O5114.08 (5)O9—C21—H21B109.5
O3—Pr1—O569.08 (5)H21A—C21—H21B109.5
O4—Pr1—O685.38 (5)O9—C21—H21C109.5
O2—Pr1—O6137.30 (5)H21A—C21—H21C109.5
O3—Pr1—O6135.46 (5)H21B—C21—H21C109.5
O5—Pr1—O668.67 (5)F2B—C1—F1A125.5 (3)
O4—Pr1—O178.05 (5)F2B—C1—F3A61.3 (3)
O2—Pr1—O167.64 (6)F1A—C1—F3A104.8 (3)
O3—Pr1—O172.17 (6)F2B—C1—F3B106.3 (4)
O5—Pr1—O1138.50 (5)F1A—C1—F3B71.2 (3)
O6—Pr1—O1140.23 (5)F3A—C1—F3B46.0 (3)
O4—Pr1—O975.46 (5)F2B—C1—F1B107.3 (3)
O2—Pr1—O9111.86 (5)F1A—C1—F1B39.5 (3)
O3—Pr1—O9132.25 (5)F3A—C1—F1B131.0 (3)
O5—Pr1—O9133.46 (5)F3B—C1—F1B110.2 (3)
O6—Pr1—O972.98 (5)F2B—C1—F2A43.2 (3)
O1—Pr1—O967.97 (5)F1A—C1—F2A107.2 (3)
O4—Pr1—O8136.78 (5)F3A—C1—F2A103.2 (3)
O2—Pr1—O874.39 (5)F3B—C1—F2A143.1 (3)
O3—Pr1—O8148.64 (5)F1B—C1—F2A72.3 (3)
O5—Pr1—O8123.32 (5)F2B—C1—C2114.7 (3)
O6—Pr1—O870.66 (5)F1A—C1—C2118.0 (3)
O1—Pr1—O897.65 (5)F3A—C1—C2115.7 (2)
O9—Pr1—O863.52 (5)F3B—C1—C2106.1 (3)
O4—Pr1—O7145.50 (5)F1B—C1—C2112.0 (3)
O2—Pr1—O766.19 (6)F2A—C1—C2106.5 (2)
O3—Pr1—O7101.52 (5)F6—C5—F4107.0 (2)
O5—Pr1—O769.98 (5)F6—C5—F5106.2 (2)
O6—Pr1—O776.54 (6)F4—C5—F5106.8 (2)
O1—Pr1—O7133.29 (5)F6—C5—C4110.9 (2)
O9—Pr1—O7124.82 (5)F4—C5—C4111.71 (19)
O8—Pr1—O763.39 (5)F5—C5—C4113.9 (2)
C2—O1—Pr1136.62 (15)F9B—C6—F9A57.9 (4)
C4—O2—Pr1138.77 (15)F9B—C6—F8B106.0 (2)
C7—O3—Pr1134.04 (14)F9A—C6—F8B51.2 (3)
C9—O4—Pr1134.85 (14)F9B—C6—F7A55.4 (4)
C12—O5—Pr1136.88 (13)F9A—C6—F7A112.0 (5)
C14—O6—Pr1135.01 (13)F8B—C6—F7A145.3 (4)
C16—O7—C17111.2 (2)F9B—C6—F8A139.9 (5)
C16—O7—Pr1118.21 (14)F9A—C6—F8A107.5 (5)
C17—O7—Pr1115.37 (13)F8B—C6—F8A58.9 (4)
C19—O8—C18111.89 (17)F7A—C6—F8A114.0 (6)
C19—O8—Pr1115.94 (14)F9B—C6—F7B106.5 (2)
C18—O8—Pr1116.57 (13)F9A—C6—F7B134.9 (4)
C20—O9—C21110.60 (19)F8B—C6—F7B107.7 (2)
C20—O9—Pr1115.26 (15)F7A—C6—F7B59.9 (4)
C21—O9—Pr1123.35 (13)F8A—C6—F7B54.6 (4)
O1—C2—C3127.8 (2)F9B—C6—C7112.35 (18)
O1—C2—C1114.2 (2)F9A—C6—C7111.3 (4)
C3—C2—C1118.02 (19)F8B—C6—C7110.1 (2)
C2—C3—C4121.0 (2)F7A—C6—C7104.3 (3)
C2—C3—H3119.5F8A—C6—C7107.7 (5)
C4—C3—H3119.5F7B—C6—C7113.7 (2)
O2—C4—C3127.2 (2)F12B—C10—F11A129.4 (3)
O2—C4—C5114.06 (19)F12B—C10—F10B112.6 (3)
C3—C4—C5118.69 (19)F11A—C10—F10B61.3 (3)
O3—C7—C8126.7 (2)F12B—C10—F12A37.5 (3)
O3—C7—C6113.3 (2)F11A—C10—F12A105.3 (3)
C8—C7—C6120.0 (2)F10B—C10—F12A131.7 (3)
C7—C8—C9126.3 (2)F12B—C10—F11B104.6 (3)
C7—C8—H8116.9F11A—C10—F11B43.2 (2)
C9—C8—H8116.9F10B—C10—F11B103.0 (3)
O4—C9—C8126.4 (2)F12A—C10—F11B69.1 (2)
O4—C9—C10113.93 (18)F12B—C10—F10A66.1 (3)
C8—C9—C10119.7 (2)F11A—C10—F10A108.5 (3)
O5—C12—C13128.07 (19)F10B—C10—F10A52.1 (2)
O5—C12—C11114.85 (17)F12A—C10—F10A100.3 (2)
C13—C12—C11117.08 (17)F11B—C10—F10A137.0 (3)
C12—C13—C14121.01 (18)F12B—C10—C9114.1 (3)
C12—C13—H13119.5F11A—C10—C9113.3 (2)
C14—C13—H13119.5F10B—C10—C9113.3 (3)
O6—C14—C13128.53 (18)F12A—C10—C9114.4 (2)
O6—C14—C15114.52 (18)F11B—C10—C9108.0 (2)
C13—C14—C15116.94 (18)F10A—C10—C9114.0 (2)
O7—C16—H16A109.5F14B—C11—F13A132.7 (3)
O7—C16—H16B109.5F14B—C11—F15B108.2 (3)
H16A—C16—H16B109.5F13A—C11—F15B65.3 (3)
O7—C16—H16C109.5F14B—C11—F15A69.9 (2)
H16A—C16—H16C109.5F13A—C11—F15A105.6 (3)
H16B—C16—H16C109.5F15B—C11—F15A43.1 (2)
O7—C17—C18108.4 (2)F14B—C11—F14A41.9 (2)
O7—C17—H17A110.0F13A—C11—F14A105.8 (3)
C18—C17—H17A110.0F15B—C11—F14A132.7 (3)
O7—C17—H17B110.0F15A—C11—F14A108.2 (3)
C18—C17—H17B110.0F14B—C11—F13B110.3 (3)
H17A—C17—H17B108.4F13A—C11—F13B42.9 (2)
O8—C18—C17109.04 (18)F15B—C11—F13B106.9 (3)
O8—C18—H18A109.9F15A—C11—F13B139.5 (3)
C17—C18—H18A109.9F14A—C11—F13B70.2 (3)
O8—C18—H18B109.9F14B—C11—C12112.8 (2)
C17—C18—H18B109.9F13A—C11—C12112.7 (2)
H18A—C18—H18B108.3F15B—C11—C12111.5 (2)
O8—C19—C20108.16 (19)F15A—C11—C12109.7 (2)
O8—C19—H19A110.1F14A—C11—C12114.3 (2)
C20—C19—H19A110.1F13B—C11—C12107.1 (2)
O8—C19—H19B110.1F17—C15—F16107.1 (2)
C20—C19—H19B110.1F17—C15—F18104.4 (2)
H19A—C19—H19B108.4F16—C15—F18104.5 (2)
O9—C20—C19109.01 (19)F17—C15—C14112.7 (2)
O9—C20—H20A109.9F16—C15—C14115.1 (2)
C19—C20—H20A109.9F18—C15—C14112.3 (2)
O4—Pr1—O1—C2144.0 (2)O7—Pr1—O9—C21175.63 (16)
O2—Pr1—O1—C210.1 (2)Pr1—O1—C2—C39.6 (4)
O3—Pr1—O1—C269.8 (2)Pr1—O1—C2—C1170.84 (15)
O5—Pr1—O1—C291.5 (2)O1—C2—C3—C40.4 (4)
O6—Pr1—O1—C2148.56 (19)C1—C2—C3—C4180.0 (2)
O9—Pr1—O1—C2137.1 (2)Pr1—O2—C4—C34.5 (4)
O8—Pr1—O1—C279.7 (2)Pr1—O2—C4—C5174.54 (15)
O7—Pr1—O1—C219.3 (2)C2—C3—C4—O22.2 (4)
O4—Pr1—O2—C431.3 (2)C2—C3—C4—C5178.7 (2)
O3—Pr1—O2—C469.0 (2)Pr1—O3—C7—C84.8 (3)
O5—Pr1—O2—C4126.9 (2)Pr1—O3—C7—C6176.95 (12)
O6—Pr1—O2—C4149.04 (19)O3—C7—C8—C90.4 (4)
O1—Pr1—O2—C47.8 (2)C6—C7—C8—C9177.7 (2)
O9—Pr1—O2—C460.8 (2)Pr1—O4—C9—C81.9 (3)
O8—Pr1—O2—C4113.1 (2)Pr1—O4—C9—C10179.59 (12)
O7—Pr1—O2—C4179.5 (2)C7—C8—C9—O41.9 (4)
O4—Pr1—O3—C75.42 (18)C7—C8—C9—C10175.6 (2)
O2—Pr1—O3—C7159.48 (19)Pr1—O5—C12—C138.3 (4)
O5—Pr1—O3—C776.40 (18)Pr1—O5—C12—C11170.51 (15)
O6—Pr1—O3—C757.1 (2)O5—C12—C13—C142.0 (4)
O1—Pr1—O3—C788.43 (19)C11—C12—C13—C14179.2 (2)
O9—Pr1—O3—C754.0 (2)Pr1—O6—C14—C1313.1 (4)
O8—Pr1—O3—C7163.41 (16)Pr1—O6—C14—C15168.00 (15)
O7—Pr1—O3—C7139.54 (18)C12—C13—C14—O60.6 (4)
O2—Pr1—O4—C942.4 (2)C12—C13—C14—C15179.5 (2)
O3—Pr1—O4—C94.01 (17)C16—O7—C17—C18175.21 (18)
O5—Pr1—O4—C968.22 (17)Pr1—O7—C17—C1846.60 (19)
O6—Pr1—O4—C9137.37 (17)C19—O8—C18—C17179.7 (2)
O1—Pr1—O4—C978.99 (17)Pr1—O8—C18—C1743.6 (2)
O9—Pr1—O4—C9149.04 (18)O7—C17—C18—O858.4 (2)
O8—Pr1—O4—C9167.46 (16)C18—O8—C19—C20178.8 (2)
O7—Pr1—O4—C979.35 (19)Pr1—O8—C19—C2044.2 (2)
O4—Pr1—O5—C12102.6 (2)C21—O9—C20—C19167.0 (2)
O2—Pr1—O5—C12121.4 (2)Pr1—O9—C20—C1947.3 (2)
O3—Pr1—O5—C12177.8 (2)O8—C19—C20—O959.5 (3)
O6—Pr1—O5—C1212.2 (2)O1—C2—C1—F2B40.0 (4)
O1—Pr1—O5—C12155.7 (2)C3—C2—C1—F2B140.3 (3)
O9—Pr1—O5—C1248.8 (2)O1—C2—C1—F1A153.9 (3)
O8—Pr1—O5—C1234.8 (2)C3—C2—C1—F1A25.7 (4)
O7—Pr1—O5—C1270.7 (2)O1—C2—C1—F3A28.6 (4)
O4—Pr1—O6—C1491.2 (2)C3—C2—C1—F3A151.0 (3)
O2—Pr1—O6—C1488.6 (2)O1—C2—C1—F3B77.0 (3)
O3—Pr1—O6—C1433.7 (2)C3—C2—C1—F3B102.6 (3)
O5—Pr1—O6—C1414.29 (19)O1—C2—C1—F1B162.7 (3)
O1—Pr1—O6—C14156.25 (18)C3—C2—C1—F1B17.6 (4)
O9—Pr1—O6—C14167.4 (2)O1—C2—C1—F2A85.5 (3)
O8—Pr1—O6—C14125.4 (2)C3—C2—C1—F2A94.8 (3)
O7—Pr1—O6—C1459.2 (2)O2—C4—C5—F681.6 (2)
O4—Pr1—O7—C1671.77 (18)C3—C4—C5—F697.6 (3)
O2—Pr1—O7—C1669.17 (16)O2—C4—C5—F437.6 (3)
O3—Pr1—O7—C162.21 (17)C3—C4—C5—F4143.2 (2)
O5—Pr1—O7—C1660.27 (16)O2—C4—C5—F5158.7 (2)
O6—Pr1—O7—C16132.15 (17)C3—C4—C5—F522.1 (3)
O1—Pr1—O7—C1678.49 (18)O3—C7—C6—F9B50.4 (3)
O9—Pr1—O7—C16170.06 (16)C8—C7—C6—F9B131.2 (2)
O8—Pr1—O7—C16152.98 (17)O3—C7—C6—F9A12.5 (4)
O4—Pr1—O7—C17153.06 (13)C8—C7—C6—F9A165.9 (4)
O2—Pr1—O7—C1765.99 (14)O3—C7—C6—F8B67.5 (3)
O3—Pr1—O7—C17132.95 (14)C8—C7—C6—F8B110.9 (3)
O5—Pr1—O7—C17164.57 (14)O3—C7—C6—F7A108.4 (4)
O6—Pr1—O7—C1792.69 (14)C8—C7—C6—F7A73.2 (5)
O1—Pr1—O7—C1756.68 (15)O3—C7—C6—F8A130.1 (5)
O9—Pr1—O7—C1734.90 (15)C8—C7—C6—F8A48.3 (5)
O8—Pr1—O7—C1717.82 (13)O3—C7—C6—F7B171.50 (19)
O4—Pr1—O8—C194.94 (16)C8—C7—C6—F7B10.1 (3)
O2—Pr1—O8—C19139.87 (14)O4—C9—C10—F12B60.3 (4)
O3—Pr1—O8—C19143.80 (14)C8—C9—C10—F12B121.9 (3)
O5—Pr1—O8—C19111.27 (14)O4—C9—C10—F11A101.7 (3)
O6—Pr1—O8—C1965.07 (14)C8—C9—C10—F11A76.2 (3)
O1—Pr1—O8—C1975.72 (14)O4—C9—C10—F10B169.1 (2)
O9—Pr1—O8—C1915.04 (13)C8—C9—C10—F10B8.8 (3)
O7—Pr1—O8—C19149.33 (15)O4—C9—C10—F12A19.0 (3)
O4—Pr1—O8—C18130.04 (14)C8—C9—C10—F12A163.1 (2)
O2—Pr1—O8—C1885.14 (15)O4—C9—C10—F11B55.6 (3)
O3—Pr1—O8—C1881.21 (17)C8—C9—C10—F11B122.2 (2)
O5—Pr1—O8—C1823.72 (16)O4—C9—C10—F10A133.6 (2)
O6—Pr1—O8—C1869.92 (15)C8—C9—C10—F10A48.5 (3)
O1—Pr1—O8—C18149.30 (14)O5—C12—C11—F14B148.4 (3)
O9—Pr1—O8—C18150.03 (15)C13—C12—C11—F14B32.6 (3)
O7—Pr1—O8—C1814.34 (14)O5—C12—C11—F13A44.7 (3)
O4—Pr1—O9—C20176.35 (15)C13—C12—C11—F13A134.2 (3)
O2—Pr1—O9—C2040.77 (15)O5—C12—C11—F15B26.5 (3)
O3—Pr1—O9—C20129.11 (14)C13—C12—C11—F15B154.6 (3)
O5—Pr1—O9—C20129.57 (14)O5—C12—C11—F15A72.7 (3)
O6—Pr1—O9—C2094.08 (15)C13—C12—C11—F15A108.4 (3)
O1—Pr1—O9—C2093.58 (15)O5—C12—C11—F14A165.7 (3)
O8—Pr1—O9—C2017.64 (14)C13—C12—C11—F14A13.3 (4)
O7—Pr1—O9—C2034.71 (16)O5—C12—C11—F13B90.1 (3)
O4—Pr1—O9—C2135.43 (17)C13—C12—C11—F13B88.8 (3)
O2—Pr1—O9—C21100.15 (17)O6—C14—C15—F1785.3 (3)
O3—Pr1—O9—C2111.81 (19)C13—C14—C15—F1793.7 (3)
O5—Pr1—O9—C2189.51 (18)O6—C14—C15—F16151.5 (2)
O6—Pr1—O9—C21124.99 (18)C13—C14—C15—F1629.4 (3)
O1—Pr1—O9—C2147.34 (17)O6—C14—C15—F1832.2 (3)
O8—Pr1—O9—C21158.57 (18)C13—C14—C15—F18148.7 (2)
 

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