Acta Crystallographica Section E
Acta Crystallographica
Section E CRYSTALLOGRAPHIC COMMUNICATIONS

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Crystal structures of metallocene complexes with uranium–germanium bonds

M. L. Tarlton, S. P. Kelley and J. R. Walensky

The first structural examples of complexes with uranium–germanium bonds are presented. The two complexes both have a long U—Ge bond [distances of 3.0428 (7) and 3.0523 (7) Å.

Keywords: crystal structure; actinide; germanium; main group; organometallic chemistry.

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Supporting information

	Crystallographic Information File (CIF) https://doi.org/10.1107/S2056989021011269/vm2256sup1.cif Contains datablocks 1, 2
	Structure factor file (CIF format) https://doi.org/10.1107/S2056989021011269/vm22561sup2.hkl Contains datablock 1
	Structure factor file (CIF format) https://doi.org/10.1107/S2056989021011269/vm22562sup3.hkl Contains datablock 2

CCDC references: 2117996; 2117995

checkCIF report

Key indicators

Structure: 1

Single-crystal X-ray study
T = 100 K
Mean (C-C) = 0.011 Å
Disorder in main residue
R factor = 0.045
wR factor = 0.112
Data-to-parameter ratio = 18.9

Structure: 2

Single-crystal X-ray study
T = 100 K
Mean (C-C) = 0.009 Å
Disorder in main residue
R factor = 0.041
wR factor = 0.094
Data-to-parameter ratio = 15.7

checkCIF/PLATON results

No syntax errors found



Alert level B
PLAT971_ALERT_2_B Check Calcd Resid. Dens.  0.90A   From U1              2.55 eA-3

Author Response: Likely indicates positions of superimposed symmetry- related U and I atoms caused by packing faults.


Alert level C
PLAT213_ALERT_2_C Atom F3              has ADP max/min Ratio .....        3.2 oblate
PLAT213_ALERT_2_C Atom F5              has ADP max/min Ratio .....        3.4 prolat
PLAT213_ALERT_2_C Atom F7              has ADP max/min Ratio .....        3.2 prolat
PLAT213_ALERT_2_C Atom F1A             has ADP max/min Ratio .....        3.2 oblate
PLAT220_ALERT_2_C NonSolvent   Resd 1  C   Ueq(max)/Ueq(min) Range        3.1 Ratio
PLAT220_ALERT_2_C NonSolvent   Resd 1  F   Ueq(max)/Ueq(min) Range        3.5 Ratio
PLAT234_ALERT_4_C Large Hirshfeld Difference F2       --C27      .       0.21 Ang.
PLAT234_ALERT_4_C Large Hirshfeld Difference F1A      --C27      .       0.17 Ang.
PLAT234_ALERT_4_C Large Hirshfeld Difference F2A      --C27      .       0.20 Ang.
PLAT234_ALERT_4_C Large Hirshfeld Difference F3A      --C27      .       0.16 Ang.
PLAT342_ALERT_3_C Low Bond Precision on  C-C Bonds ...............    0.01083 Ang.
PLAT420_ALERT_2_C D-H Bond Without Acceptor  Ge1      --H1       .     Please Check
PLAT601_ALERT_2_C Unit Cell Contains Solvent Accessible VOIDS of .         41 Ang   3
PLAT911_ALERT_3_C Missing FCF Refl Between Thmin & STh/L=    0.600          2 Report
PLAT971_ALERT_2_C Check Calcd Resid. Dens.  0.84A   From U1              2.02 eA-3

Author Response: Likely indicates positions of superimposed symmetry- related U and I atoms caused by packing faults.

PLAT971_ALERT_2_C Check Calcd Resid. Dens.  1.81A   From C9              1.92 eA-3

Author Response: Likely indicates positions of superimposed symmetry- related U and I atoms caused by packing faults.

PLAT971_ALERT_2_C Check Calcd Resid. Dens.  1.76A   From C20             1.68 eA-3

Author Response: Likely indicates positions of superimposed symmetry- related U and I atoms caused by packing faults.

PLAT971_ALERT_2_C Check Calcd Resid. Dens.  2.63A   From F1              1.64 eA-3

Author Response: Likely indicates positions of superimposed symmetry- related U and I atoms caused by packing faults.

PLAT972_ALERT_2_C Check Calcd Resid. Dens.  0.83A   From U1             -1.87 eA-3
PLAT972_ALERT_2_C Check Calcd Resid. Dens.  0.50A   From I1             -1.77 eA-3
PLAT972_ALERT_2_C Check Calcd Resid. Dens.  0.70A   From U1             -1.74 eA-3
PLAT972_ALERT_2_C Check Calcd Resid. Dens.  0.64A   From I1             -1.68 eA-3
PLAT972_ALERT_2_C Check Calcd Resid. Dens.  0.71A   From I1             -1.65 eA-3
PLAT972_ALERT_2_C Check Calcd Resid. Dens.  0.53A   From I1             -1.51 eA-3
PLAT973_ALERT_2_C Check Calcd Positive Resid. Density on        U1       1.44 eA-3
PLAT977_ALERT_2_C Check Negative Difference Density on H10B             -0.34 eA-3
PLAT978_ALERT_2_C Number C-C Bonds with Positive Residual Density.          0 Info

Alert level G
PLAT002_ALERT_2_G Number of Distance or Angle Restraints on AtSite         11 Note
PLAT063_ALERT_4_G Crystal Size Possibly too Large for Beam Size ..       0.64 mm
PLAT083_ALERT_2_G SHELXL Second Parameter in WGHT  Unusually Large     173.32 Why ?
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          1 Report
PLAT176_ALERT_4_G The CIF-Embedded .res File Contains SADI Records          1 Report
PLAT232_ALERT_2_G Hirshfeld Test Diff (M-X)  U1       --I1       .       11.3 s.u.
PLAT232_ALERT_2_G Hirshfeld Test Diff (M-X)  U1       --Ge1      .        8.0 s.u.
PLAT242_ALERT_2_G Low    'MainMol' Ueq as Compared to Neighbors of        C27 Check
PLAT242_ALERT_2_G Low    'MainMol' Ueq as Compared to Neighbors of        C28 Check
PLAT242_ALERT_2_G Low    'MainMol' Ueq as Compared to Neighbors of        C35 Check
PLAT242_ALERT_2_G Low    'MainMol' Ueq as Compared to Neighbors of        C36 Check
PLAT301_ALERT_3_G Main Residue  Disorder ..............(Resd  1  )         6% Note
PLAT860_ALERT_3_G Number of Least-Squares Restraints .............         24 Note
PLAT910_ALERT_3_G Missing # of FCF Reflection(s) Below Theta(Min).          4 Note
PLAT912_ALERT_4_G Missing # of FCF Reflections Above STh/L=  0.600         40 Note
PLAT933_ALERT_2_G Number of OMIT Records in Embedded .res File ...          5 Note

   0 ALERT level A = Most likely a serious problem - resolve or explain
   1 ALERT level B = A potentially serious problem, consider carefully
  27 ALERT level C = Check. Ensure it is not caused by an omission or oversight
  17 ALERT level G = General information/check it is not something unexpected

   0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
  31 ALERT type 2 Indicator that the structure model may be wrong or deficient
   5 ALERT type 3 Indicator that the structure quality may be low
   9 ALERT type 4 Improvement, methodology, query or suggestion
   0 ALERT type 5 Informative message, check




Alert level C
PLAT094_ALERT_2_C Ratio of Maximum / Minimum Residual Density ....       2.15 Report
PLAT213_ALERT_2_C Atom F6              has ADP max/min Ratio .....        3.3 prolat
PLAT213_ALERT_2_C Atom F12             has ADP max/min Ratio .....        3.2 prolat
PLAT213_ALERT_2_C Atom F13             has ADP max/min Ratio .....        3.9 prolat
PLAT213_ALERT_2_C Atom C16             has ADP max/min Ratio .....        3.3 prolat
PLAT220_ALERT_2_C NonSolvent   Resd 1  C   Ueq(max)/Ueq(min) Range        3.7 Ratio
PLAT222_ALERT_3_C NonSolvent Resd 1  H   Uiso(max)/Uiso(min) Range        4.6 Ratio
PLAT342_ALERT_3_C Low Bond Precision on  C-C Bonds ...............    0.00947 Ang.
PLAT971_ALERT_2_C Check Calcd Resid. Dens.  0.93A   From U1              1.81 eA-3
PLAT971_ALERT_2_C Check Calcd Resid. Dens.  0.81A   From U1              1.52 eA-3
PLAT978_ALERT_2_C Number C-C Bonds with Positive Residual Density.          0 Info

Alert level G
PLAT083_ALERT_2_G SHELXL Second Parameter in WGHT  Unusually Large      21.65 Why ?
PLAT232_ALERT_2_G Hirshfeld Test Diff (M-X)  U1       --F1       .        8.0 s.u.
PLAT242_ALERT_2_G Low    'MainMol' Ueq as Compared to Neighbors of        C27 Check
PLAT242_ALERT_2_G Low    'MainMol' Ueq as Compared to Neighbors of        C28 Check
PLAT242_ALERT_2_G Low    'MainMol' Ueq as Compared to Neighbors of        C35 Check
PLAT242_ALERT_2_G Low    'MainMol' Ueq as Compared to Neighbors of        C36 Check
PLAT300_ALERT_4_G Atom Site Occupancy of F11        Constrained at       0.75 Check
PLAT300_ALERT_4_G Atom Site Occupancy of F12        Constrained at       0.75 Check
PLAT300_ALERT_4_G Atom Site Occupancy of F13        Constrained at       0.75 Check
PLAT300_ALERT_4_G Atom Site Occupancy of F1A        Constrained at       0.25 Check
PLAT300_ALERT_4_G Atom Site Occupancy of F2A        Constrained at       0.25 Check
PLAT300_ALERT_4_G Atom Site Occupancy of F3A        Constrained at       0.25 Check
PLAT301_ALERT_3_G Main Residue  Disorder ..............(Resd  1  )         6% Note
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          8 Note

   0 ALERT level A = Most likely a serious problem - resolve or explain
   0 ALERT level B = A potentially serious problem, consider carefully
  11 ALERT level C = Check. Ensure it is not caused by an omission or oversight
  15 ALERT level G = General information/check it is not something unexpected

   0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
  15 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
   7 ALERT type 4 Improvement, methodology, query or suggestion
   0 ALERT type 5 Informative message, check

Computing details top

For both structures, data collection: APEX3 (Bruker, 2015); cell refinement: APEX3 and SAINT Bruker, 2015); data reduction: APEX3 and SAINT (Bruker, 2015); program(s) used to solve structure: ShelXT (Sheldrick, 2015a); program(s) used to refine structure: SHELXL (Sheldrick, 2015b); molecular graphics: OLEX2 (Dolomanov et al., 2009); software used to prepare material for publication: OLEX2 (Dolomanov et al., 2009).

Bis[3,5-bis(trifluoromethyl)phenyl-2κC¹](hydrido-2κH)(iodido-1κI)bis[1,1(η⁵)-pentamethylcyclopentadienyl]germaniumuranium(Ge—U) (1) top

Crystal data top

[GeU(C₁₀H₁₅)₂(C₈H₃F₆)₂HI]	F(000) = 4304
M_r = 1135.17	D_x = 1.908 Mg m⁻³
Monoclinic, C2/c	Mo Kα radiation, λ = 0.71073 Å
a = 23.647 (2) Å	Cell parameters from 9630 reflections
b = 21.123 (2) Å	θ = 2.3–27.5°
c = 16.8132 (18) Å	µ = 5.71 mm⁻¹
β = 109.727 (3)°	T = 100 K
V = 7905.1 (14) Å³	Block, clear dark red
Z = 8	0.64 × 0.63 × 0.53 mm

Data collection top

Bruker VENTURE CMOS area detector diffractometer	9105 independent reflections
Radiation source: Incoatec IMuS microfocus Mo tube	7700 reflections with I > 2σ(I)
Mirror optics monochromator	R_int = 0.076
shutterless ω and phi scans	θ_max = 27.6°, θ_min = 2.1°
Absorption correction: multi-scan (AXScale; Bruker, 2015	h = −30→30
T_min = 0.136, T_max = 0.563	k = −27→27
103146 measured reflections	l = −21→21

Refinement top

Refinement on F²	Primary atom site location: dual
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F² > 2σ(F²)] = 0.045	Hydrogen site location: mixed
wR(F²) = 0.112	H atoms treated by a mixture of independent and constrained refinement
S = 1.03	w = 1/[σ²(F_o²) + (0.0386P)² + 173.3198P] where P = (F_o² + 2F_c²)/3
9105 reflections	(Δ/σ)_max = 0.001
483 parameters	Δρ_max = 2.63 e Å⁻³
24 restraints	Δρ_min = −2.00 e Å⁻³

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

	x	y	z	U_iso*/U_eq	Occ. (<1)
U1	0.18303 (2)	0.40289 (2)	0.22613 (2)	0.02210 (7)
I1	0.19437 (2)	0.46585 (3)	0.07554 (3)	0.04105 (13)
Ge1	0.23147 (3)	0.52325 (3)	0.32511 (4)	0.02585 (15)
H1	0.246 (4)	0.520 (4)	0.426 (5)	0.039*
F1A	0.4365 (6)	0.6046 (11)	0.5595 (9)	0.109 (4)	0.464 (8)
F1	0.4744 (9)	0.5657 (7)	0.5371 (13)	0.110 (7)	0.536 (8)
F2A	0.5027 (9)	0.5735 (9)	0.5113 (16)	0.110 (7)	0.464 (8)
F2	0.4384 (7)	0.6600 (7)	0.5192 (10)	0.109 (5)	0.536 (8)
F3A	0.4751 (10)	0.6698 (7)	0.5007 (12)	0.109 (5)	0.464 (8)
F3	0.5061 (5)	0.6352 (9)	0.4725 (8)	0.109 (4)	0.536 (8)
F4	0.4282 (4)	0.6384 (4)	0.1750 (7)	0.129 (4)
F5	0.3490 (4)	0.5935 (8)	0.1099 (6)	0.190 (7)
F6	0.4288 (5)	0.5425 (4)	0.1679 (7)	0.137 (4)
F7	0.1194 (3)	0.7214 (5)	0.4377 (4)	0.117 (3)
F8	0.0405 (3)	0.6758 (3)	0.3649 (5)	0.087 (2)
F9	0.0577 (3)	0.7667 (3)	0.3300 (4)	0.0722 (17)
F10	0.1741 (2)	0.6968 (3)	0.0655 (3)	0.0534 (12)
F11	0.1048 (3)	0.7579 (3)	0.0734 (3)	0.0630 (14)
F12	0.0850 (3)	0.6622 (3)	0.0332 (3)	0.0694 (17)
C1	0.0722 (3)	0.3493 (3)	0.1721 (4)	0.0279 (13)
C2	0.0639 (3)	0.4093 (3)	0.1313 (4)	0.0285 (13)
C3	0.0723 (2)	0.4567 (3)	0.1946 (4)	0.0252 (13)
C4	0.0858 (3)	0.4259 (3)	0.2733 (4)	0.0276 (13)
C5	0.0854 (3)	0.3593 (3)	0.2592 (4)	0.0284 (13)
C6	0.0613 (3)	0.2873 (3)	0.1245 (5)	0.0399 (17)
H6A	0.063316	0.252425	0.163798	0.060*
H6B	0.091982	0.281264	0.097991	0.060*
H6C	0.021438	0.288026	0.080787	0.060*
C7	0.0410 (3)	0.4208 (4)	0.0382 (5)	0.0377 (16)
H7A	−0.003004	0.419826	0.017583	0.056*
H7B	0.056238	0.387892	0.009666	0.056*
H7C	0.054762	0.462383	0.026230	0.056*
C8	0.0588 (3)	0.5254 (3)	0.1753 (5)	0.0340 (15)
H8A	0.015918	0.530556	0.143154	0.051*
H8B	0.082587	0.541203	0.141780	0.051*
H8C	0.068911	0.549283	0.228180	0.051*
C9	0.0943 (3)	0.4553 (4)	0.3573 (5)	0.0394 (17)
H9A	0.097478	0.501394	0.353127	0.059*
H9B	0.131085	0.438836	0.399139	0.059*
H9C	0.059806	0.445118	0.374915	0.059*
C10	0.0858 (3)	0.3111 (4)	0.3250 (5)	0.0396 (17)
H10A	0.048729	0.314808	0.338548	0.059*
H10B	0.120489	0.318517	0.376143	0.059*
H10C	0.088414	0.268562	0.303315	0.059*
C11	0.2315 (3)	0.2881 (3)	0.2742 (5)	0.0392 (17)
C12	0.2580 (3)	0.3278 (3)	0.3464 (5)	0.0351 (15)
C13	0.2977 (3)	0.3702 (3)	0.3269 (5)	0.0320 (15)
C14	0.2950 (3)	0.3581 (4)	0.2433 (5)	0.0387 (17)
C15	0.2536 (3)	0.3084 (4)	0.2096 (5)	0.0398 (17)
C16	0.1953 (3)	0.2293 (4)	0.2722 (7)	0.053 (2)
H16A	0.163938	0.225434	0.216741	0.079*
H16B	0.176690	0.231989	0.316107	0.079*
H16C	0.221698	0.192246	0.282553	0.079*
C17	0.2496 (4)	0.3238 (4)	0.4304 (5)	0.050 (2)
H17A	0.288641	0.317533	0.474717	0.075*
H17B	0.223126	0.288127	0.430502	0.075*
H17C	0.231464	0.363186	0.441232	0.075*
C18	0.3429 (3)	0.4092 (4)	0.3919 (6)	0.049 (2)
H18A	0.322576	0.434577	0.423024	0.073*
H18B	0.363414	0.437359	0.364152	0.073*
H18C	0.372367	0.381303	0.431330	0.073*
C19	0.3359 (4)	0.3871 (5)	0.2017 (7)	0.062 (3)
H19A	0.338664	0.432828	0.212015	0.093*
H19B	0.319838	0.379129	0.140729	0.093*
H19C	0.376000	0.368182	0.225204	0.093*
C20	0.2392 (4)	0.2778 (5)	0.1243 (6)	0.060 (3)
H20A	0.258735	0.301474	0.090570	0.089*
H20B	0.195631	0.277903	0.095305	0.089*
H20C	0.253939	0.234074	0.131298	0.089*
C21	0.3109 (3)	0.5558 (3)	0.3272 (5)	0.0298 (14)
C22	0.3540 (3)	0.5740 (4)	0.4035 (5)	0.0409 (17)
H22	0.344913	0.571929	0.454317	0.049*
C23	0.4105 (3)	0.5953 (4)	0.4056 (7)	0.049 (2)
C24	0.4240 (3)	0.6000 (4)	0.3321 (7)	0.056 (3)
H24	0.462479	0.614503	0.333896	0.067*
C25	0.3812 (3)	0.5835 (4)	0.2557 (6)	0.049 (2)
C26	0.3249 (3)	0.5609 (3)	0.2540 (5)	0.0378 (16)
H26	0.295972	0.548802	0.201613	0.045*
C27	0.4564 (4)	0.6116 (4)	0.4879 (7)	0.075 (4)
C28	0.3955 (4)	0.5882 (5)	0.1769 (8)	0.067 (3)
C29	0.1829 (3)	0.6014 (3)	0.2877 (4)	0.0241 (12)
C30	0.1740 (3)	0.6265 (3)	0.2080 (4)	0.0271 (13)
H30	0.193921	0.607524	0.173506	0.033*
C31	0.1371 (3)	0.6781 (3)	0.1772 (4)	0.0273 (13)
C32	0.1080 (3)	0.7072 (3)	0.2261 (4)	0.0314 (14)
H32	0.082281	0.742376	0.205070	0.038*
C33	0.1171 (3)	0.6837 (3)	0.3066 (5)	0.0318 (14)
C34	0.1543 (3)	0.6318 (3)	0.3374 (4)	0.0291 (13)
H34	0.160344	0.616920	0.393001	0.035*
C35	0.1250 (3)	0.6995 (3)	0.0884 (5)	0.0351 (15)
C36	0.0855 (4)	0.7132 (4)	0.3606 (5)	0.048 (2)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
U1	0.01205 (11)	0.02461 (12)	0.02617 (13)	0.00298 (8)	0.00192 (8)	0.00320 (9)
I1	0.0379 (3)	0.0551 (3)	0.0289 (2)	0.0017 (2)	0.00962 (19)	0.0068 (2)
Ge1	0.0192 (3)	0.0290 (3)	0.0281 (3)	−0.0005 (2)	0.0064 (3)	0.0019 (3)
F1A	0.052 (5)	0.174 (14)	0.077 (7)	−0.054 (7)	−0.008 (5)	−0.034 (8)
F1	0.105 (16)	0.094 (8)	0.081 (13)	0.008 (10)	−0.032 (10)	−0.004 (7)
F2A	0.105 (16)	0.094 (8)	0.081 (13)	0.008 (10)	−0.032 (10)	−0.004 (7)
F2	0.126 (15)	0.090 (8)	0.080 (9)	−0.032 (9)	−0.007 (10)	−0.034 (7)
F3A	0.126 (15)	0.090 (8)	0.080 (9)	−0.032 (9)	−0.007 (10)	−0.034 (7)
F3	0.052 (5)	0.174 (14)	0.077 (7)	−0.054 (7)	−0.008 (5)	−0.034 (8)
F4	0.155 (8)	0.091 (5)	0.198 (10)	−0.015 (5)	0.134 (8)	0.022 (6)
F5	0.074 (6)	0.43 (2)	0.077 (6)	−0.021 (8)	0.043 (5)	0.056 (9)
F6	0.210 (11)	0.092 (6)	0.172 (9)	0.036 (6)	0.149 (9)	0.006 (6)
F7	0.087 (5)	0.207 (9)	0.042 (3)	0.078 (5)	0.002 (3)	−0.042 (4)
F8	0.079 (4)	0.100 (5)	0.114 (5)	0.016 (4)	0.073 (4)	0.013 (4)
F9	0.091 (4)	0.065 (4)	0.074 (4)	0.043 (3)	0.045 (3)	0.008 (3)
F10	0.045 (3)	0.079 (4)	0.039 (3)	−0.005 (2)	0.018 (2)	0.013 (2)
F11	0.078 (4)	0.053 (3)	0.055 (3)	0.016 (3)	0.019 (3)	0.024 (2)
F12	0.069 (4)	0.084 (4)	0.034 (3)	−0.047 (3)	−0.010 (2)	0.002 (2)
C1	0.015 (3)	0.024 (3)	0.041 (4)	−0.002 (2)	0.004 (3)	0.000 (3)
C2	0.014 (3)	0.034 (3)	0.032 (3)	0.001 (2)	0.002 (2)	0.001 (3)
C3	0.006 (2)	0.028 (3)	0.035 (3)	0.001 (2)	−0.003 (2)	0.001 (3)
C4	0.010 (3)	0.037 (3)	0.035 (3)	0.007 (2)	0.006 (2)	0.000 (3)
C5	0.012 (3)	0.036 (3)	0.035 (4)	−0.004 (2)	0.005 (2)	0.006 (3)
C6	0.026 (3)	0.033 (4)	0.053 (5)	0.002 (3)	0.003 (3)	−0.005 (3)
C7	0.025 (3)	0.044 (4)	0.032 (4)	0.002 (3)	−0.006 (3)	0.002 (3)
C8	0.018 (3)	0.026 (3)	0.048 (4)	−0.001 (2)	−0.002 (3)	0.000 (3)
C9	0.027 (3)	0.055 (5)	0.037 (4)	0.000 (3)	0.012 (3)	−0.011 (3)
C10	0.029 (4)	0.045 (4)	0.046 (4)	0.000 (3)	0.014 (3)	0.012 (3)
C11	0.023 (3)	0.027 (3)	0.059 (5)	0.002 (3)	0.002 (3)	−0.002 (3)
C12	0.029 (3)	0.025 (3)	0.045 (4)	0.006 (3)	0.005 (3)	0.009 (3)
C13	0.014 (3)	0.027 (3)	0.047 (4)	0.009 (2)	−0.001 (3)	0.008 (3)
C14	0.018 (3)	0.042 (4)	0.057 (5)	0.011 (3)	0.013 (3)	0.009 (3)
C15	0.022 (3)	0.042 (4)	0.051 (4)	0.016 (3)	0.006 (3)	−0.005 (3)
C16	0.029 (4)	0.028 (4)	0.092 (7)	0.008 (3)	0.007 (4)	0.008 (4)
C17	0.045 (5)	0.056 (5)	0.041 (4)	0.013 (4)	0.005 (4)	0.016 (4)
C18	0.022 (3)	0.037 (4)	0.065 (6)	0.005 (3)	−0.015 (3)	0.006 (4)
C19	0.035 (4)	0.072 (6)	0.087 (7)	0.018 (4)	0.032 (5)	0.023 (5)
C20	0.051 (5)	0.063 (6)	0.059 (6)	0.022 (4)	0.010 (4)	−0.018 (5)
C21	0.016 (3)	0.025 (3)	0.042 (4)	0.002 (2)	0.001 (3)	0.000 (3)
C22	0.028 (4)	0.034 (4)	0.050 (5)	0.003 (3)	−0.001 (3)	−0.003 (3)
C23	0.018 (3)	0.035 (4)	0.081 (7)	0.000 (3)	−0.002 (4)	−0.007 (4)
C24	0.017 (3)	0.044 (5)	0.102 (8)	−0.001 (3)	0.013 (4)	0.001 (5)
C25	0.024 (4)	0.046 (5)	0.080 (6)	0.007 (3)	0.022 (4)	0.011 (4)
C26	0.020 (3)	0.032 (4)	0.061 (5)	0.004 (3)	0.013 (3)	0.002 (3)
C27	0.034 (5)	0.054 (6)	0.113 (10)	−0.010 (4)	−0.006 (5)	−0.024 (6)
C28	0.043 (5)	0.071 (7)	0.099 (9)	−0.001 (5)	0.044 (6)	0.009 (6)
C29	0.015 (3)	0.025 (3)	0.033 (3)	−0.002 (2)	0.008 (2)	−0.003 (2)
C30	0.020 (3)	0.030 (3)	0.033 (3)	−0.008 (2)	0.010 (3)	−0.003 (3)
C31	0.020 (3)	0.031 (3)	0.027 (3)	−0.010 (2)	0.003 (2)	−0.001 (2)
C32	0.019 (3)	0.033 (3)	0.037 (4)	−0.002 (3)	0.002 (3)	−0.001 (3)
C33	0.024 (3)	0.031 (3)	0.038 (4)	−0.002 (3)	0.008 (3)	−0.003 (3)
C34	0.023 (3)	0.034 (3)	0.029 (3)	−0.003 (3)	0.007 (3)	0.002 (3)
C35	0.031 (4)	0.035 (4)	0.036 (4)	−0.008 (3)	0.006 (3)	0.009 (3)
C36	0.043 (4)	0.064 (5)	0.045 (5)	0.012 (4)	0.024 (4)	0.003 (4)

Geometric parameters (Å, º) top

U1—I1	2.9511 (6)	C9—H9C	0.9800
U1—Ge1	3.0428 (7)	C10—H10A	0.9800
U1—C1	2.714 (6)	C10—H10B	0.9800
U1—C2	2.731 (6)	C10—H10C	0.9800
U1—C3	2.738 (6)	C11—C12	1.434 (11)
U1—C4	2.718 (6)	C11—C15	1.420 (12)
U1—C5	2.712 (6)	C11—C16	1.502 (10)
U1—C11	2.686 (7)	C12—C13	1.413 (10)
U1—C12	2.707 (7)	C12—C17	1.494 (11)
U1—C13	2.756 (6)	C13—C14	1.411 (11)
U1—C14	2.735 (6)	C13—C18	1.492 (10)
U1—C15	2.674 (7)	C14—C15	1.418 (11)
Ge1—H1	1.61 (8)	C14—C19	1.501 (11)
Ge1—C21	1.990 (6)	C15—C20	1.505 (12)
Ge1—C29	1.988 (6)	C16—H16A	0.9800
F1A—C27	1.440 (14)	C16—H16B	0.9800
F1—C27	1.252 (14)	C16—H16C	0.9800
F2A—C27	1.307 (15)	C17—H17A	0.9800
F2—C27	1.285 (13)	C17—H17B	0.9800
F3A—C27	1.298 (13)	C17—H17C	0.9800
F3—C27	1.379 (12)	C18—H18A	0.9800
F4—C28	1.318 (10)	C18—H18B	0.9800
F5—C28	1.287 (12)	C18—H18C	0.9800
F6—C28	1.287 (10)	C19—H19A	0.9800
F7—C36	1.285 (10)	C19—H19B	0.9800
F8—C36	1.348 (11)	C19—H19C	0.9800
F9—C36	1.321 (10)	C20—H20A	0.9800
F10—C35	1.341 (9)	C20—H20B	0.9800
F11—C35	1.315 (9)	C20—H20C	0.9800
F12—C35	1.336 (8)	C21—C22	1.396 (10)
C1—C2	1.422 (9)	C21—C26	1.382 (11)
C1—C5	1.406 (10)	C22—H22	0.9500
C1—C6	1.511 (9)	C22—C23	1.397 (11)
C2—C3	1.426 (9)	C23—C24	1.382 (15)
C2—C7	1.494 (10)	C23—C27	1.484 (13)
C3—C4	1.411 (9)	C24—H24	0.9500
C3—C8	1.497 (9)	C24—C25	1.386 (14)
C4—C5	1.425 (10)	C25—C26	1.404 (10)
C4—C9	1.494 (10)	C25—C28	1.477 (14)
C5—C10	1.502 (9)	C26—H26	0.9500
C6—H6A	0.9800	C29—C30	1.389 (9)
C6—H6B	0.9800	C29—C34	1.397 (9)
C6—H6C	0.9800	C30—H30	0.9500
C7—H7A	0.9800	C30—C31	1.382 (9)
C7—H7B	0.9800	C31—C32	1.383 (9)
C7—H7C	0.9800	C31—C35	1.493 (9)
C8—H8A	0.9800	C32—H32	0.9500
C8—H8B	0.9800	C32—C33	1.388 (10)
C8—H8C	0.9800	C33—C34	1.391 (9)
C9—H9A	0.9800	C33—C36	1.492 (10)
C9—H9B	0.9800	C34—H34	0.9500

I1—U1—Ge1	88.063 (19)	H10A—C10—H10B	109.5
C1—U1—I1	104.96 (15)	H10A—C10—H10C	109.5
C1—U1—Ge1	132.39 (14)	H10B—C10—H10C	109.5
C1—U1—C2	30.28 (19)	C12—C11—U1	75.4 (4)
C1—U1—C3	49.91 (18)	C12—C11—C16	125.8 (8)
C1—U1—C4	49.9 (2)	C15—C11—U1	74.2 (4)
C1—U1—C13	137.69 (19)	C15—C11—C12	107.6 (6)
C1—U1—C14	133.0 (2)	C15—C11—C16	125.9 (8)
C2—U1—I1	81.46 (14)	C16—C11—U1	123.9 (5)
C2—U1—Ge1	113.68 (14)	C11—C12—U1	73.8 (4)
C2—U1—C3	30.23 (19)	C11—C12—C17	127.4 (7)
C2—U1—C13	167.88 (19)	C13—C12—U1	76.9 (4)
C2—U1—C14	148.2 (2)	C13—C12—C11	108.0 (7)
C3—U1—I1	90.27 (14)	C13—C12—C17	124.5 (7)
C3—U1—Ge1	85.29 (13)	C17—C12—U1	118.5 (5)
C3—U1—C13	154.3 (2)	C12—C13—U1	73.1 (4)
C4—U1—I1	120.04 (14)	C12—C13—C18	123.2 (7)
C4—U1—Ge1	83.71 (14)	C14—C13—U1	74.3 (4)
C4—U1—C2	49.8 (2)	C14—C13—C12	107.9 (6)
C4—U1—C3	29.97 (19)	C14—C13—C18	127.6 (7)
C4—U1—C13	128.2 (2)	C18—C13—U1	128.7 (4)
C4—U1—C14	156.4 (2)	C13—C14—U1	76.0 (4)
C5—U1—I1	131.23 (14)	C13—C14—C15	108.9 (7)
C5—U1—Ge1	111.14 (15)	C13—C14—C19	124.9 (8)
C5—U1—C1	30.0 (2)	C15—C14—U1	72.5 (4)
C5—U1—C2	49.8 (2)	C15—C14—C19	125.7 (8)
C5—U1—C3	49.87 (19)	C19—C14—U1	124.3 (5)
C5—U1—C4	30.4 (2)	C11—C15—U1	75.1 (4)
C5—U1—C13	121.2 (2)	C11—C15—C20	125.2 (8)
C5—U1—C14	136.3 (2)	C14—C15—U1	77.2 (4)
C11—U1—I1	120.78 (18)	C14—C15—C11	107.6 (7)
C11—U1—Ge1	123.07 (16)	C14—C15—C20	127.0 (8)
C11—U1—C1	89.4 (2)	C20—C15—U1	118.2 (5)
C11—U1—C2	118.1 (2)	C11—C16—H16A	109.5
C11—U1—C3	135.7 (2)	C11—C16—H16B	109.5
C11—U1—C4	113.0 (2)	C11—C16—H16C	109.5
C11—U1—C5	86.5 (2)	H16A—C16—H16B	109.5
C11—U1—C12	30.8 (2)	H16A—C16—H16C	109.5
C11—U1—C13	50.1 (2)	H16B—C16—H16C	109.5
C11—U1—C14	50.0 (2)	C12—C17—H17A	109.5
C12—U1—I1	132.74 (16)	C12—C17—H17B	109.5
C12—U1—Ge1	92.87 (16)	C12—C17—H17C	109.5
C12—U1—C1	108.7 (2)	H17A—C17—H17B	109.5
C12—U1—C2	138.7 (2)	H17A—C17—H17C	109.5
C12—U1—C3	136.9 (2)	H17B—C17—H17C	109.5
C12—U1—C4	107.0 (2)	C13—C18—H18A	109.5
C12—U1—C5	92.1 (2)	C13—C18—H18B	109.5
C12—U1—C13	30.0 (2)	C13—C18—H18C	109.5
C12—U1—C14	49.6 (2)	H18A—C18—H18B	109.5
C13—U1—I1	106.56 (15)	H18A—C18—H18C	109.5
C13—U1—Ge1	76.24 (14)	H18B—C18—H18C	109.5
C14—U1—I1	83.15 (17)	C14—C19—H19A	109.5
C14—U1—Ge1	93.36 (17)	C14—C19—H19B	109.5
C14—U1—C3	173.3 (2)	C14—C19—H19C	109.5
C14—U1—C13	29.8 (2)	H19A—C19—H19B	109.5
C15—U1—I1	90.39 (18)	H19A—C19—H19C	109.5
C15—U1—Ge1	123.18 (17)	H19B—C19—H19C	109.5
C15—U1—C1	102.7 (2)	C15—C20—H20A	109.5
C15—U1—C2	122.2 (2)	C15—C20—H20B	109.5
C15—U1—C3	151.5 (2)	C15—C20—H20C	109.5
C15—U1—C4	141.5 (2)	H20A—C20—H20B	109.5
C15—U1—C5	111.9 (2)	H20A—C20—H20C	109.5
C15—U1—C11	30.7 (3)	H20B—C20—H20C	109.5
C15—U1—C12	50.7 (2)	C22—C21—Ge1	120.2 (6)
C15—U1—C13	50.1 (2)	C26—C21—Ge1	121.3 (5)
C15—U1—C14	30.4 (2)	C26—C21—C22	118.5 (7)
U1—Ge1—H1	117 (3)	C21—C22—H22	119.8
C21—Ge1—U1	118.5 (2)	C21—C22—C23	120.4 (8)
C21—Ge1—H1	97 (3)	C23—C22—H22	119.8
C29—Ge1—U1	116.73 (18)	C22—C23—C27	119.4 (9)
C29—Ge1—H1	105 (3)	C24—C23—C22	120.6 (8)
C29—Ge1—C21	99.2 (2)	C24—C23—C27	120.0 (8)
C2—C1—U1	75.5 (3)	C23—C24—H24	120.2
C2—C1—C6	123.0 (6)	C23—C24—C25	119.5 (7)
C5—C1—U1	74.9 (3)	C25—C24—H24	120.2
C5—C1—C2	108.3 (6)	C24—C25—C26	119.7 (9)
C5—C1—C6	128.4 (6)	C24—C25—C28	119.7 (8)
C6—C1—U1	120.8 (4)	C26—C25—C28	120.5 (9)
C1—C2—U1	74.2 (3)	C21—C26—C25	121.2 (8)
C1—C2—C3	107.7 (6)	C21—C26—H26	119.4
C1—C2—C7	126.4 (6)	C25—C26—H26	119.4
C3—C2—U1	75.1 (3)	F1A—C27—C23	114.3 (9)
C3—C2—C7	125.2 (6)	F1—C27—F2	115.5 (13)
C7—C2—U1	123.9 (4)	F1—C27—F3	106.4 (11)
C2—C3—U1	74.6 (3)	F1—C27—C23	114.5 (12)
C2—C3—C8	123.6 (6)	F2A—C27—F1A	99.3 (12)
C4—C3—U1	74.2 (3)	F2A—C27—C23	114.3 (14)
C4—C3—C2	107.8 (6)	F2—C27—F3	102.2 (10)
C4—C3—C8	127.9 (6)	F2—C27—C23	109.0 (10)
C8—C3—U1	124.4 (4)	F3A—C27—F1A	98.6 (11)
C3—C4—U1	75.8 (3)	F3A—C27—F2A	109.2 (12)
C3—C4—C5	108.2 (6)	F3A—C27—C23	118.4 (12)
C3—C4—C9	127.7 (6)	F3—C27—C23	108.1 (10)
C5—C4—U1	74.6 (3)	F4—C28—C25	113.0 (10)
C5—C4—C9	124.0 (6)	F5—C28—F4	104.1 (11)
C9—C4—U1	119.6 (4)	F5—C28—C25	113.8 (7)
C1—C5—U1	75.1 (3)	F6—C28—F4	102.3 (8)
C1—C5—C4	108.0 (6)	F6—C28—F5	109.8 (12)
C1—C5—C10	127.5 (6)	F6—C28—C25	112.9 (9)
C4—C5—U1	75.0 (3)	C30—C29—Ge1	120.3 (5)
C4—C5—C10	123.3 (6)	C30—C29—C34	117.1 (6)
C10—C5—U1	126.0 (4)	C34—C29—Ge1	122.5 (5)
C1—C6—H6A	109.5	C29—C30—H30	118.9
C1—C6—H6B	109.5	C31—C30—C29	122.2 (6)
C1—C6—H6C	109.5	C31—C30—H30	118.9
H6A—C6—H6B	109.5	C30—C31—C32	120.4 (6)
H6A—C6—H6C	109.5	C30—C31—C35	119.9 (6)
H6B—C6—H6C	109.5	C32—C31—C35	119.6 (6)
C2—C7—H7A	109.5	C31—C32—H32	120.8
C2—C7—H7B	109.5	C31—C32—C33	118.5 (6)
C2—C7—H7C	109.5	C33—C32—H32	120.8
H7A—C7—H7B	109.5	C32—C33—C34	121.0 (6)
H7A—C7—H7C	109.5	C32—C33—C36	120.0 (7)
H7B—C7—H7C	109.5	C34—C33—C36	119.0 (7)
C3—C8—H8A	109.5	C29—C34—H34	119.6
C3—C8—H8B	109.5	C33—C34—C29	120.8 (6)
C3—C8—H8C	109.5	C33—C34—H34	119.6
H8A—C8—H8B	109.5	F10—C35—C31	112.4 (6)
H8A—C8—H8C	109.5	F11—C35—F10	106.2 (6)
H8B—C8—H8C	109.5	F11—C35—F12	107.1 (6)
C4—C9—H9A	109.5	F11—C35—C31	114.3 (7)
C4—C9—H9B	109.5	F12—C35—F10	104.7 (6)
C4—C9—H9C	109.5	F12—C35—C31	111.5 (5)
H9A—C9—H9B	109.5	F7—C36—F8	105.1 (8)
H9A—C9—H9C	109.5	F7—C36—F9	109.7 (8)
H9B—C9—H9C	109.5	F7—C36—C33	113.6 (7)
C5—C10—H10A	109.5	F8—C36—C33	110.8 (7)
C5—C10—H10B	109.5	F9—C36—F8	102.8 (7)
C5—C10—H10C	109.5	F9—C36—C33	114.0 (7)

Bis[3,5-bis(trifluoromethyl)phenyl-2κC¹](fluorido-1κI)(hydrido-2κH)bis[1,1(η⁵)-pentamethylcyclopentadienyl]germaniumuranium(Ge—U) (2) top

Crystal data top

[GeU(C₁₀H₁₅)₂(C₈H₃F₆)₂FH]	F(000) = 4016
M_r = 1041.30	D_x = 1.844 Mg m⁻³
Monoclinic, C2/c	Mo Kα radiation, λ = 0.71073 Å
a = 34.160 (3) Å	Cell parameters from 9918 reflections
b = 13.5237 (11) Å	θ = 2.3–23.3°
c = 16.2986 (13) Å	µ = 5.21 mm⁻¹
β = 95.028 (2)°	T = 100 K
V = 7500.4 (10) Å³	Prism, clear dark red
Z = 8	0.10 × 0.10 × 0.08 mm

Data collection top

Bruker APEXII CCD diffractometer	5563 reflections with I > 2σ(I)
φ and ω scans	R_int = 0.081
Absorption correction: multi-scan (SADABS; Bruker, 2015)	θ_max = 26.5°, θ_min = 1.6°
T_min = 0.501, T_max = 0.562	h = −42→42
65643 measured reflections	k = −16→16
7720 independent reflections	l = −20→20

Refinement top

Refinement on F²	Primary atom site location: dual
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F² > 2σ(F²)] = 0.041	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.094	H-atom parameters constrained
S = 1.05	w = 1/[σ²(F_o²) + (0.0441P)² + 21.6495P] where P = (F_o² + 2F_c²)/3
7720 reflections	(Δ/σ)_max = 0.001
492 parameters	Δρ_max = 1.68 e Å⁻³
0 restraints	Δρ_min = −0.78 e Å⁻³

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

	x	y	z	U_iso*/U_eq	Occ. (<1)
U1	0.37698 (2)	0.91030 (2)	0.40571 (2)	0.03137 (8)
Ge1	0.34983 (2)	0.70121 (4)	0.35878 (4)	0.02943 (15)
F1	0.38083 (14)	0.9430 (4)	0.2718 (3)	0.0798 (14)
F1A	0.4259 (6)	0.6888 (19)	0.0809 (14)	0.059 (7)*	0.25
F2	0.36774 (11)	0.6810 (3)	0.6963 (2)	0.0528 (10)
F2A	0.4111 (7)	0.5508 (19)	0.0457 (14)	0.070 (6)*	0.25
F3	0.30596 (11)	0.7033 (3)	0.6925 (2)	0.0527 (10)
F3A	0.4673 (6)	0.5837 (17)	0.0875 (12)	0.064 (5)*	0.25
F4	0.33071 (13)	0.5681 (3)	0.7388 (2)	0.0590 (11)
F5	0.2643 (2)	0.3420 (4)	0.5447 (4)	0.125 (3)
F6	0.30011 (16)	0.3142 (4)	0.4505 (5)	0.128 (3)
F7	0.24878 (18)	0.3913 (4)	0.4284 (4)	0.106 (2)
F8	0.42298 (13)	0.3341 (3)	0.3844 (3)	0.0679 (13)
F9	0.45845 (18)	0.3155 (4)	0.2866 (3)	0.102 (2)
F10	0.47779 (16)	0.4025 (4)	0.3882 (4)	0.103 (2)
F11	0.39263 (19)	0.6235 (7)	0.0486 (3)	0.088 (2)	0.75
F12	0.4469 (3)	0.6813 (7)	0.0902 (4)	0.089 (3)	0.75
F13	0.4411 (4)	0.5303 (5)	0.0554 (4)	0.102 (3)	0.75
C1	0.30338 (17)	0.9809 (5)	0.3689 (4)	0.0377 (15)
C2	0.30009 (17)	0.9202 (5)	0.4381 (4)	0.0359 (14)
C3	0.32110 (17)	0.9643 (5)	0.5051 (4)	0.0349 (15)
C4	0.33680 (19)	1.0537 (5)	0.4790 (5)	0.0451 (17)
C5	0.3263 (2)	1.0616 (5)	0.3930 (5)	0.0456 (18)
C6	0.28286 (19)	0.9627 (6)	0.2847 (4)	0.057 (2)
H6A	0.302274	0.944506	0.246500	0.086*
H6B	0.269101	1.022952	0.265059	0.086*
H6C	0.263849	0.908854	0.287715	0.086*
C7	0.27336 (17)	0.8335 (5)	0.4455 (5)	0.0482 (18)
H7A	0.264189	0.809488	0.390379	0.072*
H7B	0.250742	0.853633	0.474574	0.072*
H7C	0.287652	0.780550	0.476327	0.072*
C8	0.3214 (2)	0.9282 (6)	0.5923 (4)	0.0526 (19)
H8A	0.330927	0.859888	0.595617	0.079*
H8B	0.294675	0.930990	0.609746	0.079*
H8C	0.338746	0.970290	0.628403	0.079*
C9	0.3541 (2)	1.1334 (6)	0.5340 (6)	0.077 (3)
H9A	0.369275	1.103688	0.581581	0.115*
H9B	0.333002	1.174235	0.553025	0.115*
H9C	0.371460	1.174702	0.503573	0.115*
C10	0.3358 (3)	1.1463 (6)	0.3375 (6)	0.076 (3)
H10A	0.356864	1.186643	0.365227	0.114*
H10B	0.312351	1.187129	0.325362	0.114*
H10C	0.344460	1.119977	0.286069	0.114*
C11	0.45358 (18)	0.9564 (6)	0.4048 (5)	0.0511 (19)
C12	0.45269 (17)	0.8548 (6)	0.4005 (4)	0.0464 (18)
C13	0.44244 (16)	0.8168 (5)	0.4758 (4)	0.0367 (15)
C14	0.43624 (16)	0.8966 (5)	0.5274 (4)	0.0374 (15)
C15	0.44352 (18)	0.9842 (5)	0.4837 (5)	0.0457 (17)
C16	0.4660 (2)	1.0261 (9)	0.3402 (6)	0.110 (4)
H16A	0.459523	0.997306	0.285517	0.165*
H16B	0.494410	1.037220	0.348837	0.165*
H16C	0.452177	1.089153	0.344149	0.165*
C17	0.4655 (2)	0.7930 (8)	0.3298 (5)	0.090 (3)
H17A	0.456631	0.724666	0.335665	0.135*
H17B	0.494219	0.794334	0.330707	0.135*
H17C	0.453917	0.820165	0.277461	0.135*
C18	0.4437 (2)	0.7100 (5)	0.5018 (5)	0.065 (2)
H18A	0.426927	0.700429	0.546950	0.097*
H18B	0.470798	0.691613	0.520396	0.097*
H18C	0.434235	0.668309	0.455030	0.097*
C19	0.4270 (2)	0.8889 (7)	0.6161 (4)	0.064 (2)
H19A	0.420021	0.954337	0.636099	0.096*
H19B	0.450102	0.863895	0.649682	0.096*
H19C	0.404921	0.843410	0.620074	0.096*
C20	0.4470 (2)	1.0879 (6)	0.5166 (7)	0.084 (3)
H20A	0.430763	1.132280	0.480334	0.126*
H20B	0.474508	1.109160	0.518893	0.126*
H20C	0.438032	1.089872	0.572071	0.126*
C21	0.33441 (17)	0.6153 (4)	0.4498 (4)	0.0304 (13)
C22	0.34129 (16)	0.6465 (4)	0.5310 (4)	0.0298 (13)
H22	0.355005	0.706794	0.542250	0.036*
C23	0.32877 (16)	0.5925 (4)	0.5960 (4)	0.0298 (13)
C24	0.30822 (17)	0.5052 (4)	0.5809 (4)	0.0355 (15)
H24	0.299070	0.468129	0.624861	0.043*
C25	0.30132 (17)	0.4732 (4)	0.5005 (4)	0.0331 (14)
C26	0.31381 (16)	0.5275 (4)	0.4362 (4)	0.0325 (14)
H26	0.308182	0.504397	0.381438	0.039*
C27	0.33361 (18)	0.6341 (5)	0.6810 (4)	0.0374 (15)
C28	0.2795 (2)	0.3801 (5)	0.4824 (5)	0.0458 (17)
C29	0.38704 (17)	0.6139 (4)	0.3047 (4)	0.0322 (14)
C30	0.40422 (16)	0.5301 (4)	0.3407 (4)	0.0313 (13)
H30	0.399218	0.513209	0.395424	0.038*
C31	0.42879 (17)	0.4699 (4)	0.2982 (4)	0.0328 (14)
C32	0.43653 (18)	0.4931 (5)	0.2190 (4)	0.0353 (14)
H32	0.453532	0.452673	0.190272	0.042*
C33	0.41927 (19)	0.5758 (4)	0.1818 (4)	0.0345 (14)
C34	0.39482 (17)	0.6349 (5)	0.2230 (4)	0.0338 (14)
H34	0.382949	0.691027	0.196017	0.041*
C35	0.4467 (2)	0.3801 (5)	0.3383 (4)	0.0454 (17)
C36	0.4265 (2)	0.6010 (5)	0.0957 (4)	0.0425 (16)
C37	0.30396 (19)	0.6882 (5)	0.2750 (4)	0.0440 (16)
H37A	0.280389	0.714353	0.297535	0.066*
H37B	0.299901	0.618264	0.260811	0.066*
H37C	0.309036	0.725430	0.225470	0.066*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
U1	0.02538 (11)	0.02903 (13)	0.04074 (15)	0.00002 (10)	0.00874 (9)	−0.00207 (11)
Ge1	0.0341 (3)	0.0281 (3)	0.0267 (3)	0.0022 (3)	0.0062 (3)	−0.0023 (3)
F1	0.068 (3)	0.100 (4)	0.073 (3)	0.009 (3)	0.013 (3)	0.026 (3)
F2	0.055 (2)	0.060 (3)	0.041 (2)	−0.015 (2)	−0.0021 (19)	−0.0006 (19)
F3	0.062 (2)	0.059 (3)	0.037 (2)	0.007 (2)	0.0064 (19)	−0.0077 (19)
F4	0.080 (3)	0.059 (3)	0.037 (2)	−0.015 (2)	−0.001 (2)	0.0139 (19)
F5	0.205 (7)	0.088 (4)	0.089 (4)	−0.099 (5)	0.049 (4)	−0.022 (3)
F6	0.082 (4)	0.048 (3)	0.262 (8)	−0.015 (3)	0.061 (5)	−0.070 (4)
F7	0.100 (4)	0.062 (3)	0.147 (5)	−0.034 (3)	−0.036 (4)	−0.004 (3)
F8	0.081 (3)	0.050 (3)	0.077 (3)	0.022 (2)	0.034 (3)	0.026 (2)
F9	0.168 (5)	0.081 (4)	0.064 (3)	0.086 (4)	0.049 (3)	0.023 (3)
F10	0.073 (3)	0.101 (4)	0.127 (5)	0.010 (3)	−0.035 (3)	0.042 (4)
F11	0.061 (4)	0.172 (8)	0.032 (3)	0.016 (5)	0.009 (3)	0.036 (4)
F12	0.114 (7)	0.113 (7)	0.041 (4)	−0.080 (6)	0.015 (4)	0.012 (4)
F13	0.217 (10)	0.063 (5)	0.037 (4)	0.080 (6)	0.062 (5)	0.019 (3)
C1	0.030 (3)	0.048 (4)	0.037 (4)	0.014 (3)	0.013 (3)	0.014 (3)
C2	0.030 (3)	0.039 (4)	0.041 (4)	0.004 (3)	0.014 (3)	0.002 (3)
C3	0.038 (3)	0.038 (4)	0.031 (4)	0.013 (3)	0.015 (3)	0.002 (3)
C4	0.037 (3)	0.030 (3)	0.070 (5)	0.005 (3)	0.013 (3)	−0.008 (3)
C5	0.045 (4)	0.039 (4)	0.056 (5)	0.010 (3)	0.021 (3)	0.017 (3)
C6	0.038 (4)	0.097 (6)	0.038 (4)	0.022 (4)	0.009 (3)	0.017 (4)
C7	0.028 (3)	0.051 (4)	0.069 (5)	0.000 (3)	0.021 (3)	0.004 (4)
C8	0.057 (4)	0.068 (5)	0.035 (4)	0.022 (4)	0.019 (3)	0.003 (3)
C9	0.064 (5)	0.059 (5)	0.108 (8)	0.007 (4)	0.012 (5)	−0.043 (5)
C10	0.093 (6)	0.039 (5)	0.102 (7)	0.019 (4)	0.048 (6)	0.036 (5)
C11	0.026 (3)	0.081 (6)	0.046 (5)	−0.016 (4)	0.002 (3)	0.021 (4)
C12	0.023 (3)	0.073 (6)	0.044 (4)	−0.001 (3)	0.007 (3)	−0.011 (4)
C13	0.021 (3)	0.038 (4)	0.051 (4)	0.005 (3)	0.002 (3)	−0.002 (3)
C14	0.025 (3)	0.053 (4)	0.034 (4)	0.003 (3)	0.001 (3)	−0.006 (3)
C15	0.032 (3)	0.034 (4)	0.069 (5)	−0.009 (3)	−0.006 (3)	−0.002 (4)
C16	0.059 (5)	0.167 (11)	0.102 (8)	−0.059 (6)	−0.010 (5)	0.080 (8)
C17	0.037 (4)	0.169 (10)	0.067 (6)	0.005 (5)	0.018 (4)	−0.049 (6)
C18	0.045 (4)	0.041 (4)	0.103 (7)	0.010 (3)	−0.021 (4)	0.003 (4)
C19	0.042 (4)	0.112 (7)	0.036 (4)	0.004 (4)	−0.003 (3)	−0.001 (4)
C20	0.047 (4)	0.047 (5)	0.151 (9)	−0.004 (4)	−0.033 (5)	−0.021 (5)
C21	0.031 (3)	0.029 (3)	0.032 (3)	0.002 (2)	0.006 (3)	0.000 (3)
C22	0.032 (3)	0.026 (3)	0.032 (3)	0.000 (2)	0.005 (3)	−0.002 (3)
C23	0.029 (3)	0.028 (3)	0.033 (3)	0.000 (3)	0.004 (2)	0.002 (3)
C24	0.032 (3)	0.033 (3)	0.043 (4)	0.001 (3)	0.011 (3)	0.006 (3)
C25	0.035 (3)	0.023 (3)	0.042 (4)	0.002 (3)	0.011 (3)	−0.005 (3)
C26	0.037 (3)	0.029 (3)	0.032 (3)	0.003 (3)	0.008 (3)	−0.006 (3)
C27	0.039 (3)	0.035 (4)	0.037 (4)	−0.004 (3)	−0.003 (3)	0.007 (3)
C28	0.053 (4)	0.026 (3)	0.059 (5)	−0.003 (3)	0.012 (4)	−0.004 (3)
C29	0.039 (3)	0.025 (3)	0.034 (4)	−0.004 (3)	0.010 (3)	−0.011 (3)
C30	0.038 (3)	0.034 (3)	0.023 (3)	−0.001 (3)	0.009 (3)	−0.001 (3)
C31	0.036 (3)	0.033 (3)	0.030 (3)	0.000 (3)	0.008 (3)	0.000 (3)
C32	0.040 (3)	0.035 (4)	0.033 (4)	0.004 (3)	0.012 (3)	−0.006 (3)
C33	0.047 (4)	0.030 (3)	0.028 (3)	−0.003 (3)	0.009 (3)	−0.001 (3)
C34	0.041 (3)	0.030 (3)	0.031 (4)	0.004 (3)	0.009 (3)	−0.002 (3)
C35	0.050 (4)	0.053 (4)	0.035 (4)	0.014 (3)	0.011 (3)	0.006 (3)
C36	0.064 (5)	0.031 (4)	0.034 (4)	0.000 (4)	0.018 (3)	−0.004 (3)
C37	0.049 (4)	0.046 (4)	0.037 (4)	0.010 (3)	0.002 (3)	−0.004 (3)

Geometric parameters (Å, º) top

U1—F1	2.243 (5)	C10—H10B	0.9800
U1—C5	2.676 (6)	C10—H10C	0.9800
U1—C11	2.691 (6)	C11—C12	1.375 (11)
U1—C15	2.697 (6)	C11—C15	1.411 (10)
U1—C12	2.701 (6)	C11—C16	1.501 (10)
U1—C1	2.707 (6)	C12—C13	1.403 (9)
U1—C3	2.710 (5)	C12—C17	1.519 (10)
U1—C4	2.712 (6)	C13—C14	1.396 (9)
U1—C14	2.713 (6)	C13—C18	1.505 (9)
U1—C2	2.727 (6)	C14—C15	1.415 (9)
U1—C13	2.731 (6)	C14—C19	1.510 (9)
U1—Ge1	3.0524 (7)	C15—C20	1.502 (10)
Ge1—C21	1.991 (6)	C16—H16A	0.9800
Ge1—C37	1.994 (6)	C16—H16B	0.9800
Ge1—C29	1.996 (6)	C16—H16C	0.9800
F1A—C36	1.21 (2)	C17—H17A	0.9800
F2—C27	1.331 (7)	C17—H17B	0.9800
F2A—C36	1.15 (2)	C17—H17C	0.9800
F3—C27	1.354 (7)	C18—H18A	0.9800
F3A—C36	1.43 (2)	C18—H18B	0.9800
F4—C27	1.308 (7)	C18—H18C	0.9800
F5—C28	1.288 (8)	C19—H19A	0.9800
F6—C28	1.274 (8)	C19—H19B	0.9800
F7—C28	1.319 (9)	C19—H19C	0.9800
F8—C35	1.309 (8)	C20—H20A	0.9800
F9—C35	1.302 (8)	C20—H20B	0.9800
F10—C35	1.315 (8)	C20—H20C	0.9800
F11—C36	1.367 (9)	C21—C26	1.388 (8)
F12—C36	1.296 (9)	C21—C22	1.389 (8)
F13—C36	1.284 (8)	C22—C23	1.386 (8)
C1—C5	1.381 (9)	C22—H22	0.9500
C1—C2	1.407 (8)	C23—C24	1.384 (8)
C1—C6	1.506 (9)	C23—C27	1.491 (9)
C2—C3	1.388 (9)	C24—C25	1.380 (8)
C2—C7	1.498 (9)	C24—H24	0.9500
C3—C4	1.403 (9)	C25—C26	1.377 (8)
C3—C8	1.502 (9)	C25—C28	1.479 (9)
C4—C5	1.419 (10)	C26—H26	0.9500
C4—C9	1.491 (10)	C29—C30	1.383 (8)
C5—C10	1.512 (9)	C29—C34	1.410 (8)
C6—H6A	0.9800	C30—C31	1.397 (8)
C6—H6B	0.9800	C30—H30	0.9500
C6—H6C	0.9800	C31—C32	1.377 (8)
C7—H7A	0.9800	C31—C35	1.485 (9)
C7—H7B	0.9800	C32—C33	1.379 (8)
C7—H7C	0.9800	C32—H32	0.9500
C8—H8A	0.9800	C33—C34	1.374 (8)
C8—H8B	0.9800	C33—C36	1.486 (9)
C8—H8C	0.9800	C34—H34	0.9500
C9—H9A	0.9800	C37—H37A	0.9800
C9—H9B	0.9800	C37—H37B	0.9800
C9—H9C	0.9800	C37—H37C	0.9800
C10—H10A	0.9800

F1—U1—C5	82.3 (2)	C12—C11—C15	107.8 (6)
F1—U1—C11	78.98 (19)	C12—C11—C16	126.7 (9)
C5—U1—C11	116.4 (2)	C15—C11—C16	125.3 (9)
F1—U1—C15	105.5 (2)	C12—C11—U1	75.6 (4)
C5—U1—C15	105.4 (2)	C15—C11—U1	75.0 (3)
C11—U1—C15	30.4 (2)	C16—C11—U1	118.9 (5)
F1—U1—C12	83.48 (19)	C11—C12—C13	109.2 (6)
C5—U1—C12	145.5 (2)	C11—C12—C17	125.5 (8)
C11—U1—C12	29.5 (2)	C13—C12—C17	124.9 (8)
C15—U1—C12	49.3 (2)	C11—C12—U1	74.8 (4)
F1—U1—C1	81.23 (17)	C13—C12—U1	76.2 (3)
C5—U1—C1	29.7 (2)	C17—C12—U1	121.1 (4)
C11—U1—C1	143.3 (2)	C14—C13—C12	107.8 (6)
C15—U1—C1	134.6 (2)	C14—C13—C18	125.1 (7)
C12—U1—C1	164.6 (2)	C12—C13—C18	126.5 (7)
F1—U1—C3	129.29 (18)	C14—C13—U1	74.5 (3)
C5—U1—C3	49.87 (19)	C12—C13—U1	73.9 (4)
C11—U1—C3	132.6 (2)	C18—C13—U1	124.4 (4)
C15—U1—C3	103.1 (2)	C13—C14—C15	107.5 (6)
C12—U1—C3	145.1 (2)	C13—C14—C19	125.4 (7)
C1—U1—C3	49.31 (18)	C15—C14—C19	126.9 (7)
F1—U1—C4	111.3 (2)	C13—C14—U1	75.8 (3)
C5—U1—C4	30.5 (2)	C15—C14—U1	74.2 (4)
C11—U1—C4	111.5 (2)	C19—C14—U1	120.0 (4)
C15—U1—C4	88.0 (2)	C11—C15—C14	107.7 (6)
C12—U1—C4	137.3 (2)	C11—C15—C20	123.8 (8)
C1—U1—C4	49.4 (2)	C14—C15—C20	127.8 (8)
C3—U1—C4	29.99 (19)	C11—C15—U1	74.6 (4)
F1—U1—C14	128.42 (18)	C14—C15—U1	75.5 (3)
C5—U1—C14	123.0 (2)	C20—C15—U1	123.5 (5)
C11—U1—C14	49.9 (2)	C11—C16—H16A	109.5
C15—U1—C14	30.33 (19)	C11—C16—H16B	109.5
C12—U1—C14	49.38 (19)	H16A—C16—H16B	109.5
C1—U1—C14	143.59 (19)	C11—C16—H16C	109.5
C3—U1—C14	95.79 (18)	H16A—C16—H16C	109.5
C4—U1—C14	95.8 (2)	H16B—C16—H16C	109.5
F1—U1—C2	108.56 (18)	C12—C17—H17A	109.5
C5—U1—C2	49.49 (19)	C12—C17—H17B	109.5
C11—U1—C2	160.6 (2)	H17A—C17—H17B	109.5
C15—U1—C2	132.6 (2)	C12—C17—H17C	109.5
C12—U1—C2	163.9 (2)	H17A—C17—H17C	109.5
C1—U1—C2	30.00 (18)	H17B—C17—H17C	109.5
C3—U1—C2	29.58 (18)	C13—C18—H18A	109.5
C4—U1—C2	49.20 (19)	C13—C18—H18B	109.5
C14—U1—C2	122.10 (19)	H18A—C18—H18B	109.5
F1—U1—C13	112.51 (18)	C13—C18—H18C	109.5
C5—U1—C13	152.4 (2)	H18A—C18—H18C	109.5
C11—U1—C13	49.4 (2)	H18B—C18—H18C	109.5
C15—U1—C13	49.38 (19)	C14—C19—H19A	109.5
C12—U1—C13	29.9 (2)	C14—C19—H19B	109.5
C1—U1—C13	165.14 (19)	H19A—C19—H19B	109.5
C3—U1—C13	117.94 (19)	C14—C19—H19C	109.5
C4—U1—C13	125.0 (2)	H19A—C19—H19C	109.5
C14—U1—C13	29.71 (18)	H19B—C19—H19C	109.5
C2—U1—C13	135.15 (19)	C15—C20—H20A	109.5
F1—U1—Ge1	88.92 (14)	C15—C20—H20B	109.5
C5—U1—Ge1	120.59 (16)	H20A—C20—H20B	109.5
C11—U1—Ge1	119.17 (19)	C15—C20—H20C	109.5
C15—U1—Ge1	133.34 (14)	H20A—C20—H20C	109.5
C12—U1—Ge1	90.33 (16)	H20B—C20—H20C	109.5
C1—U1—Ge1	90.88 (15)	C26—C21—C22	116.9 (5)
C3—U1—Ge1	100.65 (14)	C26—C21—Ge1	123.0 (4)
C4—U1—Ge1	128.17 (14)	C22—C21—Ge1	119.9 (4)
C14—U1—Ge1	108.11 (14)	C23—C22—C21	122.0 (5)
C2—U1—Ge1	79.47 (13)	C23—C22—H22	119.0
C13—U1—Ge1	84.01 (13)	C21—C22—H22	119.0
C21—Ge1—C37	102.4 (3)	C24—C23—C22	120.0 (5)
C21—Ge1—C29	101.7 (2)	C24—C23—C27	120.1 (5)
C37—Ge1—C29	97.9 (3)	C22—C23—C27	119.6 (5)
C21—Ge1—U1	116.65 (17)	C25—C24—C23	118.5 (6)
C37—Ge1—U1	117.2 (2)	C25—C24—H24	120.7
C29—Ge1—U1	117.87 (16)	C23—C24—H24	120.7
C5—C1—C2	108.5 (6)	C26—C25—C24	121.1 (6)
C5—C1—C6	126.6 (6)	C26—C25—C28	119.1 (6)
C2—C1—C6	124.8 (6)	C24—C25—C28	119.8 (6)
C5—C1—U1	73.9 (4)	C25—C26—C21	121.4 (6)
C2—C1—U1	75.8 (3)	C25—C26—H26	119.3
C6—C1—U1	119.6 (4)	C21—C26—H26	119.3
C3—C2—C1	107.9 (6)	F4—C27—F2	108.1 (5)
C3—C2—C7	123.3 (6)	F4—C27—F3	105.9 (5)
C1—C2—C7	127.9 (6)	F2—C27—F3	104.8 (5)
C3—C2—U1	74.5 (3)	F4—C27—C23	113.8 (5)
C1—C2—U1	74.2 (3)	F2—C27—C23	112.2 (5)
C7—C2—U1	125.6 (4)	F3—C27—C23	111.6 (5)
C2—C3—C4	108.5 (6)	F6—C28—F5	108.5 (7)
C2—C3—C8	124.4 (6)	F6—C28—F7	104.0 (7)
C4—C3—C8	126.6 (6)	F5—C28—F7	102.6 (7)
C2—C3—U1	75.9 (3)	F6—C28—C25	113.0 (6)
C4—C3—U1	75.1 (3)	F5—C28—C25	114.5 (6)
C8—C3—U1	122.1 (4)	F7—C28—C25	113.2 (6)
C3—C4—C5	107.1 (6)	C30—C29—C34	117.3 (5)
C3—C4—C9	125.6 (7)	C30—C29—Ge1	124.1 (4)
C5—C4—C9	126.2 (7)	C34—C29—Ge1	118.5 (4)
C3—C4—U1	74.9 (3)	C29—C30—C31	121.2 (5)
C5—C4—U1	73.3 (4)	C29—C30—H30	119.4
C9—C4—U1	126.3 (5)	C31—C30—H30	119.4
C1—C5—C4	108.0 (6)	C32—C31—C30	120.4 (6)
C1—C5—C10	125.1 (7)	C32—C31—C35	119.6 (5)
C4—C5—C10	126.8 (7)	C30—C31—C35	120.0 (5)
C1—C5—U1	76.4 (4)	C31—C32—C33	119.2 (5)
C4—C5—U1	76.2 (4)	C31—C32—H32	120.4
C10—C5—U1	117.0 (5)	C33—C32—H32	120.4
C1—C6—H6A	109.5	C34—C33—C32	120.8 (6)
C1—C6—H6B	109.5	C34—C33—C36	119.2 (6)
H6A—C6—H6B	109.5	C32—C33—C36	120.0 (5)
C1—C6—H6C	109.5	C33—C34—C29	121.2 (6)
H6A—C6—H6C	109.5	C33—C34—H34	119.4
H6B—C6—H6C	109.5	C29—C34—H34	119.4
C2—C7—H7A	109.5	F9—C35—F8	107.1 (6)
C2—C7—H7B	109.5	F9—C35—F10	106.0 (6)
H7A—C7—H7B	109.5	F8—C35—F10	105.2 (6)
C2—C7—H7C	109.5	F9—C35—C31	113.7 (6)
H7A—C7—H7C	109.5	F8—C35—C31	113.0 (5)
H7B—C7—H7C	109.5	F10—C35—C31	111.3 (6)
C3—C8—H8A	109.5	F2A—C36—F1A	115.9 (18)
C3—C8—H8B	109.5	F13—C36—F12	110.8 (8)
H8A—C8—H8B	109.5	F13—C36—F11	103.0 (7)
C3—C8—H8C	109.5	F12—C36—F11	102.0 (7)
H8A—C8—H8C	109.5	F2A—C36—F3A	103.2 (15)
H8B—C8—H8C	109.5	F1A—C36—F3A	98.2 (13)
C4—C9—H9A	109.5	F2A—C36—C33	115.4 (12)
C4—C9—H9B	109.5	F1A—C36—C33	114.2 (12)
H9A—C9—H9B	109.5	F13—C36—C33	114.6 (6)
C4—C9—H9C	109.5	F12—C36—C33	113.1 (6)
H9A—C9—H9C	109.5	F11—C36—C33	112.2 (6)
H9B—C9—H9C	109.5	F3A—C36—C33	107.2 (10)
C5—C10—H10A	109.5	Ge1—C37—H37A	109.5
C5—C10—H10B	109.5	Ge1—C37—H37B	109.5
H10A—C10—H10B	109.5	H37A—C37—H37B	109.5
C5—C10—H10C	109.5	Ge1—C37—H37C	109.5
H10A—C10—H10C	109.5	H37A—C37—H37C	109.5
H10B—C10—H10C	109.5	H37B—C37—H37C	109.5

Selected geometric parameters (Å, °) for 1 and 2 top

Parameter	1	2
U1—Ge1	3.0428 (7)	3.0524 (7)
U1—Ge1—C21	118.5 (2)	116.65 (17)
U1—Ge1—C29	116.73 (18)	117.87 (16)

top

Contact	Distance (D···A)	Distance (D—H···A)
1
Ge1—H···I1	4.5876 (9)	3.16 (8)
C7—H···F12	3.314 (9)	2.524
C16—H···C30	3.70 (1)	2.79
C20B—H···F7	3.44 (1)	2.65

2
C7—H···F3	3.403 (8)	2.652
C7—H···C24	3.536 (9)	2.863
C7···C7	3.36 (1)
C10—H···F3	3.216 (8)	2.617
C16—H···C19	3.84 (1)	2.87
C18—H···F10	3.446 (8)	2.543
C20—H···C11	3.57 (1)	2.80
C20—H···C12	3.654 (9)	2.752

H···A distances involving riding H atoms are rounded to the precision of the D···A distance.

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