#------------------------------------------------------------------------------
#$Date: 2016-03-21 18:22:36 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178810 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/64/4106473.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4106473
loop_
_publ_author_name
'Skye Fortier'
'Justin R. Walensky'
'Guang Wu'
'Trevor W. Hayton'
_publ_contact_author_email       hayton@chem.ucsb.edu
_publ_contact_author_name        'Trevor W. Hayton'
_publ_section_title
;
 High-Valent Uranium Alkyls: Evidence for the Formation of UVI(CH2SiMe3)6
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11732
_journal_page_last               11743
_journal_paper_doi               10.1021/ja204151v
_journal_volume                  133
_journal_year                    2011
_chemical_formula_sum            'C32 H40 Li O8 Si3 U'
_chemical_formula_weight         881.88
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           163
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-P 3 2c'
_symmetry_space_group_name_H-M   'P -3 1 c'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            2
_cell_length_a                   13.0591(16)
_cell_length_b                   13.0591(16)
_cell_length_c                   16.136(4)
_cell_measurement_temperature    150(2)
_cell_volume                     2383.2(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.966
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'omega scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0776
_diffrn_reflns_av_sigmaI/netI    0.0396
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            16705
_diffrn_reflns_theta_full        27.42
_diffrn_reflns_theta_max         27.42
_diffrn_reflns_theta_min         1.80
_exptl_absorpt_coefficient_mu    3.515
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.416551
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.229
_exptl_crystal_description       plate
_exptl_crystal_F_000             866
_exptl_crystal_size_max          0.7
_exptl_crystal_size_mid          0.7
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.175
_refine_diff_density_min         -0.963
_refine_diff_density_rms         0.155
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.308
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     96
_refine_ls_number_reflns         1757
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.308
_refine_ls_R_factor_all          0.0419
_refine_ls_R_factor_gt           0.0355
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0479P)²+2.8623P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1002
_refine_ls_wR_factor_ref         0.1038
_reflns_number_gt                1527
_reflns_number_total             1757
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja204151v_si_001_2.cif
_cod_data_source_block           Complex_2
_cod_database_code               4106473
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-y, -x, -z+1/2'
'-x+y, y, -z+1/2'
'x, x-y, -z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'y, x, z-1/2'
'x-y, -y, z-1/2'
'-x, -x+y, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
C7 C 0.171(5) 0.131(4) 0.369(4) 0.22(2) Uiso 0.50 1 d PD
U1 U 0.6667 0.3333 0.7500 0.02417(16) Uani 1 6 d S
Si1 Si 0.9951(2) 0.49754(12) 0.7500 0.0702(8) Uani 1 2 d S
O1 O 0.6667 0.3333 0.6208(4) 0.060(2) Uani 1 3 d S
C2 C 0.6667 0.3333 0.5332(9) 0.128(10) Uani 1 3 d S
C1 C 0.8613(9) 0.3414(12) 0.7501(12) 0.063(4) Uani 0.50 1 d P
H1A H 0.8656 0.2999 0.7987 0.075 Uiso 0.50 1 calc PR
H1B H 0.8656 0.2998 0.7016 0.075 Uiso 0.50 1 calc PR
C3 C 0.5353(15) 0.265(3) 0.5055(8) 0.194(8) Uani 1 1 d .
H3A H 0.4921 0.1969 0.5403 0.291 Uiso 1 1 calc R
H3B H 0.5306 0.2402 0.4490 0.291 Uiso 1 1 calc R
H3C H 0.5019 0.3157 0.5102 0.291 Uiso 1 1 calc R
C6 C 1.1362(14) 0.6438(12) 0.745(2) 0.103(9) Uani 0.50 1 d P
C4 C 1.004(2) 0.579(2) 0.656(2) 0.148(12) Uani 0.50 1 d P
C5 C 0.987(2) 0.414(3) 0.654(2) 0.160(14) Uani 0.50 1 d P
Li1 Li 0.0000 0.0000 0.5000 0.062(7) Uani 1 6 d S
O2 O 0.145(3) 0.014(3) 0.394(3) 0.240(19) Uani 0.50 1 d PD
O3 O 0.017(3) 0.1344(16) 0.5759(13) 0.26(2) Uani 0.50 1 d PD
C9 C -0.066(4) 0.089(4) 0.646(3) 0.21(2) Uiso 0.50 1 d PD
C10 C 0.073(3) 0.255(2) 0.545(3) 0.182(15) Uiso 0.50 1 d PD
C8 C 0.188(4) -0.045(4) 0.448(3) 0.22(2) Uiso 0.50 1 d PD
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
O3 C7 O2 74(3) 8_556 .
O3 C7 C9 80(4) 8_556 8_556
O2 C7 C9 122(4) . 8_556
O3 C7 C9 87(4) 8_556 7_556
O2 C7 C9 27(2) . 7_556
C9 C7 C9 102(5) 8_556 7_556
O3 C7 C10 59(3) 8_556 8_556
O2 C7 C10 87(3) . 8_556
C9 C7 C10 121(5) 8_556 8_556
C9 C7 C10 114(3) 7_556 8_556
O1 U1 O1 180.000(1) 4_666 .
O1 U1 C1 90.0(5) 4_666 .
O1 U1 C1 90.0(5) . .
O1 U1 C1 90.0(5) 4_666 4_666
O1 U1 C1 90.0(5) . 4_666
C1 U1 C1 64.2(6) . 4_666
O1 U1 C1 90.0(5) 4_666 3_665
O1 U1 C1 90.0(5) . 3_665
C1 U1 C1 120.000(5) . 3_665
C1 U1 C1 55.8(6) 4_666 3_665
O1 U1 C1 90.0(5) 4_666 6_556
O1 U1 C1 90.0(5) . 6_556
C1 U1 C1 55.8(6) . 6_556
C1 U1 C1 120.000(7) 4_666 6_556
C1 U1 C1 175.8(6) 3_665 6_556
O1 U1 C1 90.0(5) 4_666 2_655
O1 U1 C1 90.0(5) . 2_655
C1 U1 C1 120.000(12) . 2_655
C1 U1 C1 175.8(6) 4_666 2_655
C1 U1 C1 120.000(6) 3_665 2_655
C1 U1 C1 64.2(6) 6_556 2_655
O1 U1 C1 90.0(5) 4_666 5_656
O1 U1 C1 90.0(5) . 5_656
C1 U1 C1 175.8(6) . 5_656
C1 U1 C1 120.000(11) 4_666 5_656
C1 U1 C1 64.2(6) 3_665 5_656
C1 U1 C1 120.000(5) 6_556 5_656
C1 U1 C1 55.8(6) 2_655 5_656
C4 Si1 C4 173.3(16) . 6_556
C4 Si1 C6 67.9(12) . .
C4 Si1 C6 106.1(13) 6_556 .
C4 Si1 C6 106.1(13) . 6_556
C4 Si1 C6 67.9(12) 6_556 6_556
C6 Si1 C6 63.7(10) . 6_556
C4 Si1 C5 112.4(15) . 6_556
C4 Si1 C5 67.9(15) 6_556 6_556
C6 Si1 C5 77.4(12) . 6_556
C6 Si1 C5 107.4(13) 6_556 6_556
C4 Si1 C5 67.9(15) . .
C4 Si1 C5 112.4(15) 6_556 .
C6 Si1 C5 107.4(13) . .
C6 Si1 C5 77.4(12) 6_556 .
C5 Si1 C5 174.5(14) 6_556 .
C4 Si1 C1 73.0(11) . 6_556
C4 Si1 C1 112.6(10) 6_556 6_556
C6 Si1 C1 110.6(6) . 6_556
C6 Si1 C1 173.7(8) 6_556 6_556
C5 Si1 C1 67.8(11) 6_556 6_556
C5 Si1 C1 107.6(9) . 6_556
C4 Si1 C1 112.6(10) . .
C4 Si1 C1 73.0(11) 6_556 .
C6 Si1 C1 173.7(8) . .
C6 Si1 C1 110.6(6) 6_556 .
C5 Si1 C1 107.6(10) 6_556 .
C5 Si1 C1 67.8(11) . .
C1 Si1 C1 75.2(8) 6_556 .
C2 O1 U1 180.000(3) . .
O1 C2 C3 106.7(8) . 2_655
O1 C2 C3 106.7(8) . .
C3 C2 C3 112.1(7) 2_655 .
O1 C2 C3 106.7(8) . 3_665
C3 C2 C3 112.1(7) 2_655 3_665
C3 C2 C3 112.1(7) . 3_665
Si1 C1 U1 114.5(6) . .
Si1 C6 C6 58.1(5) . 6_556
O2 Li1 O2 180.0(14) 3 9_556
O2 Li1 O2 78.1(12) 3 2
O2 Li1 O2 101.9(12) 9_556 2
O2 Li1 O2 101.9(12) 3 7_556
O2 Li1 O2 78.1(12) 9_556 7_556
O2 Li1 O2 101.9(12) 2 7_556
O2 Li1 O2 78.1(12) 3 .
O2 Li1 O2 101.9(12) 9_556 .
O2 Li1 O2 78.1(12) 2 .
O2 Li1 O2 180.000(4) 7_556 .
O2 Li1 O2 101.9(12) 3 8_556
O2 Li1 O2 78.1(12) 9_556 8_556
O2 Li1 O2 180.000(4) 2 8_556
O2 Li1 O2 78.1(12) 7_556 8_556
O2 Li1 O2 101.9(12) . 8_556
O2 Li1 O3 53.7(11) 3 9_556
O2 Li1 O3 126.3(11) 9_556 9_556
O2 Li1 O3 37.2(13) 2 9_556
O2 Li1 O3 80.5(10) 7_556 9_556
O2 Li1 O3 99.5(10) . 9_556
O2 Li1 O3 142.8(13) 8_556 9_556
O2 Li1 O3 142.8(13) 3 .
O2 Li1 O3 37.2(13) 9_556 .
O2 Li1 O3 80.5(10) 2 .
O2 Li1 O3 53.7(11) 7_556 .
O2 Li1 O3 126.3(11) . .
O2 Li1 O3 99.5(10) 8_556 .
O3 Li1 O3 91.7(9) 9_556 .
O2 Li1 O3 99.5(10) 3 8_556
O2 Li1 O3 80.5(11) 9_556 8_556
O2 Li1 O3 53.7(11) 2 8_556
O2 Li1 O3 142.8(13) 7_556 8_556
O2 Li1 O3 37.2(13) . 8_556
O2 Li1 O3 126.3(11) 8_556 8_556
O3 Li1 O3 88.3(9) 9_556 8_556
O3 Li1 O3 91.7(9) . 8_556
O2 Li1 O3 80.5(10) 3 2
O2 Li1 O3 99.5(10) 9_556 2
O2 Li1 O3 126.3(11) 2 2
O2 Li1 O3 37.2(13) 7_556 2
O2 Li1 O3 142.8(13) . 2
O2 Li1 O3 53.7(11) 8_556 2
O3 Li1 O3 91.7(9) 9_556 2
O3 Li1 O3 88.3(9) . 2
O3 Li1 O3 180(2) 8_556 2
O2 Li1 O3 37.2(13) 3 7_556
O2 Li1 O3 142.8(13) 9_556 7_556
O2 Li1 O3 99.5(10) 2 7_556
O2 Li1 O3 126.3(11) 7_556 7_556
O2 Li1 O3 53.7(11) . 7_556
O2 Li1 O3 80.5(10) 8_556 7_556
O3 Li1 O3 88.3(9) 9_556 7_556
O3 Li1 O3 180.0(7) . 7_556
O3 Li1 O3 88.3(9) 8_556 7_556
O3 Li1 O3 91.7(9) 2 7_556
O2 Li1 O3 126.3(11) 3 3
O2 Li1 O3 53.7(11) 9_556 3
O2 Li1 O3 142.8(13) 2 3
O2 Li1 O3 99.5(10) 7_556 3
O2 Li1 O3 80.5(10) . 3
O2 Li1 O3 37.2(13) 8_556 3
O3 Li1 O3 180.000(7) 9_556 3
O3 Li1 O3 88.3(9) . 3
O3 Li1 O3 91.7(9) 8_556 3
O3 Li1 O3 88.3(9) 2 3
O3 Li1 O3 91.7(9) 7_556 3
C9 O2 C8 94(4) 7_556 .
C9 O2 C7 124(4) 7_556 .
C8 O2 C7 141(4) . .
C9 O2 O3 131(3) 7_556 8_556
C8 O2 O3 121(4) . 8_556
C7 O2 O3 39(2) . 8_556
C9 O2 Li1 94(3) 7_556 .
C8 O2 Li1 91(3) . .
C7 O2 Li1 92(3) . .
O3 O2 Li1 55.8(17) 8_556 .
C7 O3 C10 85(4) 9_556 .
C7 O3 C9 59(3) 9_556 .
C10 O3 C9 124.9(13) . .
C7 O3 O2 67(2) 9_556 9_556
C10 O3 O2 94(3) . 9_556
C9 O3 O2 107(3) . 9_556
C7 O3 Li1 146(4) 9_556 .
C10 O3 Li1 120.1(19) . .
C9 O3 Li1 112(2) . .
O2 O3 Li1 87(3) 9_556 .
O2 C9 O3 94(4) 7_556 .
O2 C9 C7 134(5) 7_556 9_556
O3 C9 C7 41(2) . 9_556
O2 C9 C8 44(2) 7_556 7_556
O3 C9 C8 82(3) . 7_556
C7 C9 C8 117(4) 9_556 7_556
O2 C9 C7 29(2) 7_556 7_556
O3 C9 C7 105(3) . 7_556
C7 C9 C7 134(4) 9_556 7_556
C8 C9 C7 73(3) 7_556 7_556
O3 C10 C8 101(3) . 2
O3 C10 C7 35.4(19) . 9_556
C8 C10 C7 136(4) 2 9_556
O2 C8 C10 137(5) . 3
O2 C8 C9 42(2) . 7_556
C10 C8 C9 136(4) 3 7_556
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C7 O3 0.98(5) 8_556
C7 O2 1.449(10) .
C7 C9 1.28(6) 8_556
C7 C9 2.50(6) 7_556
C7 C10 1.69(6) 8_556
U1 O1 2.085(7) 4_666
U1 O1 2.085(7) .
U1 C1 2.490(12) .
U1 C1 2.490(12) 4_666
U1 C1 2.490(12) 3_665
U1 C1 2.490(12) 6_556
U1 C1 2.490(12) 2_655
U1 C1 2.490(12) 5_656
Si1 C4 1.82(2) .
Si1 C4 1.82(2) 6_556
Si1 C6 1.879(15) .
Si1 C6 1.879(15) 6_556
Si1 C5 1.87(3) 6_556
Si1 C5 1.87(3) .
Si1 C1 1.910(12) 6_556
Si1 C1 1.910(13) .
O1 C2 1.414(16) .
C2 C3 1.552(15) 2_655
C2 C3 1.552(15) .
C2 C3 1.552(15) 3_665
C6 C6 1.98(3) 6_556
Li1 O2 2.49(4) 3
Li1 O2 2.49(4) 9_556
Li1 O2 2.49(4) 2
Li1 O2 2.49(4) 7_556
Li1 O2 2.49(4) .
Li1 O2 2.49(4) 8_556
Li1 O3 2.059(18) 9_556
Li1 O3 2.059(18) .
Li1 O3 2.059(18) 8_556
Li1 O3 2.059(18) 2
Li1 O3 2.059(18) 7_556
Li1 O3 2.059(18) 3
O2 C9 1.38(5) 7_556
O2 C8 1.446(10) .
O2 O3 1.51(4) 8_556
O3 C7 0.98(6) 9_556
O3 C10 1.457(10) .
O3 C9 1.466(10) .
O3 O2 1.51(4) 9_556
C9 O2 1.38(5) 7_556
C9 C7 1.28(6) 9_556
C9 C8 2.06(7) 7_556
C9 C7 2.50(6) 7_556
C10 C8 1.59(5) 2
C10 C7 1.69(6) 9_556
C8 C10 1.59(5) 3
C8 C9 2.06(7) 7_556
