#------------------------------------------------------------------------------
#$Date: 2016-03-21 18:22:36 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178810 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/64/4106475.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_4106475
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            'C40 H74 Li O9 Si4 U'
_chemical_formula_weight         1056.32
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           131
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-P 4c 2'
_symmetry_space_group_name_H-M   'P 42/m m c'
_atom_sites_solution_hydrogens   none
_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                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.3874(4)
_cell_length_b                   12.3874(4)
_cell_length_c                   19.4321(14)
_cell_measurement_temperature    150(2)
_cell_volume                     2981.8(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.961
_diffrn_measured_fraction_theta_max 0.961
_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  0.0961
_diffrn_reflns_av_sigmaI/netI    0.0392
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            23433
_diffrn_reflns_theta_full        27.42
_diffrn_reflns_theta_max         27.42
_diffrn_reflns_theta_min         2.10
_exptl_absorpt_coefficient_mu    2.840
_exptl_absorpt_correction_T_max  0.320
_exptl_absorpt_correction_T_min  0.190
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Psi Scan'
_exptl_crystal_colour            dark_red
_exptl_crystal_density_diffrn    1.177
_exptl_crystal_description       block
_exptl_crystal_F_000             1074
_exptl_crystal_size_max          1.0
_exptl_crystal_size_mid          0.6
_exptl_crystal_size_min          0.4
_refine_diff_density_max         0.767
_refine_diff_density_min         -1.039
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.177
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     102
_refine_ls_number_reflns         1836
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.210
_refine_ls_R_factor_all          0.0674
_refine_ls_R_factor_gt           0.0392
_refine_ls_shift/su_max          0.057
_refine_ls_shift/su_mean         0.010
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0464P)²+5.6043P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0973
_refine_ls_wR_factor_ref         0.1099
_reflns_number_gt                1253
_reflns_number_total             1836
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja204151v_si_001_4.cif
_cod_data_source_block           Complex_4
_cod_database_code               4106475
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'-y, x, z+1/2'
'y, -x, z+1/2'
'-x, y, -z'
'x, -y, -z'
'y, x, -z+1/2'
'-y, -x, -z+1/2'
'-x, -y, -z'
'x, y, -z'
'y, -x, -z-1/2'
'-y, x, -z-1/2'
'x, -y, z'
'-x, y, z'
'-y, -x, z-1/2'
'y, x, 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
U1 U 1.0000 0.5000 0.0000 0.02992(17) Uani 1 8 d S
Si2 Si 1.0000 0.27486(19) 0.14440(11) 0.0500(5) Uani 1 2 d S
O1 O 1.1657(6) 0.5000 0.0000 0.055(2) Uani 1 4 d S
Li1 Li 0.5000 1.0000 0.0000 0.056(7) Uani 1 8 d S
C1 C 1.2816(9) 0.5000 0.0000 0.065(4) Uani 1 4 d S
C2A C 1.0000 0.4129(13) 0.1142(8) 0.053(4) Uani 0.50 2 d SP
C2B C 1.0000 0.3184(13) 0.0555(8) 0.056(5) Uani 0.50 2 d SP
C3A C 1.0000 0.2673(19) 0.2439(9) 0.098(8) Uani 0.50 2 d SP
C3B C 1.0000 0.1181(16) 0.1489(10) 0.085(7) Uani 0.50 2 d SP
C4B C 1.1222(14) 0.3152(13) 0.1917(8) 0.083(4) Uani 0.50 1 d P
C4A C 1.1230(16) 0.2019(15) 0.1179(8) 0.115(7) Uani 0.50 1 d P
C6 C 1.3171(13) 0.4017(15) 0.0378(13) 0.145(11) Uani 0.50 1 d P
C5 C 1.320(2) 0.5000 0.0765(13) 0.094(8) Uani 0.50 2 d SP
O10 O 0.5000 0.5000 0.2500 0.28(2) Uiso 1 8 d S
C22 C 0.5000 0.388(4) 0.244(2) 0.204(19) Uiso 0.50 2 d SP
C24 C 0.383(4) 0.383(4) 0.2500 0.28(3) Uiso 0.50 2 d SP
C30 C 0.5000 1.184(3) 0.1120(18) 0.282(16) Uiso 1 2 d SD
C32 C 0.282(2) 1.076(2) 0.0488(13) 0.167(10) Uiso 0.50 1 d PD
O3 O 0.3299(13) 1.0290(15) 0.0000 0.106(6) Uiso 0.50 2 d SPD
C31 C 0.361(5) 1.103(5) 0.112(3) 0.38(4) Uiso 0.50 1 d PD
O2 O 0.4602(17) 1.1144(16) 0.0755(9) 0.177(8) 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
O1 U1 O1 180.0 . 9_765
O1 U1 C2A 90.000(1) . 10
O1 U1 C2A 90.000(1) 9_765 10
O1 U1 C2A 90.000(1) . 2_765
O1 U1 C2A 90.000(1) 9_765 2_765
C2A U1 C2A 180.0(3) 10 2_765
O1 U1 C2A 90.000(1) . 9_765
O1 U1 C2A 90.000(1) 9_765 9_765
C2A U1 C2A 51.8(7) 10 9_765
C2A U1 C2A 128.2(7) 2_765 9_765
O1 U1 C2A 90.000(1) . .
O1 U1 C2A 90.000(1) 9_765 .
C2A U1 C2A 128.2(7) 10 .
C2A U1 C2A 51.8(7) 2_765 .
C2A U1 C2A 180.0(7) 9_765 .
O1 U1 C2B 90.000(1) . 10
O1 U1 C2B 90.000(1) 9_765 10
C2A U1 C2B 38.5(5) 10 10
C2A U1 C2B 141.5(5) 2_765 10
C2A U1 C2B 90.3(5) 9_765 10
C2A U1 C2B 89.7(5) . 10
O1 U1 C2B 90.000(1) . 2_765
O1 U1 C2B 90.000(1) 9_765 2_765
C2A U1 C2B 141.5(5) 10 2_765
C2A U1 C2B 38.5(5) 2_765 2_765
C2A U1 C2B 89.7(5) 9_765 2_765
C2A U1 C2B 90.3(5) . 2_765
C2B U1 C2B 180.0(7) 10 2_765
O1 U1 C2B 90.000(1) . .
O1 U1 C2B 90.000(1) 9_765 .
C2A U1 C2B 89.7(5) 10 .
C2A U1 C2B 90.3(5) 2_765 .
C2A U1 C2B 141.5(5) 9_765 .
C2A U1 C2B 38.5(5) . .
C2B U1 C2B 51.2(7) 10 .
C2B U1 C2B 128.8(7) 2_765 .
O1 U1 C2B 90.000(1) . 9_765
O1 U1 C2B 90.000(1) 9_765 9_765
C2A U1 C2B 90.3(5) 10 9_765
C2A U1 C2B 89.7(5) 2_765 9_765
C2A U1 C2B 38.5(5) 9_765 9_765
C2A U1 C2B 141.5(5) . 9_765
C2B U1 C2B 128.8(7) 10 9_765
C2B U1 C2B 51.2(7) 2_765 9_765
C2B U1 C2B 180.0(7) . 9_765
C2A Si2 C2B 53.7(7) . .
C2A Si2 C4B 84.6(6) . .
C2B Si2 C4B 113.3(6) . .
C2A Si2 C4B 84.6(6) . 14_755
C2B Si2 C4B 113.3(6) . 14_755
C4B Si2 C4B 110.8(11) . 14_755
C2A Si2 C4A 111.9(6) . 14_755
C2B Si2 C4A 83.1(6) . 14_755
C4B Si2 C4A 162.2(7) . 14_755
C4B Si2 C4A 66.0(9) 14_755 14_755
C2A Si2 C4A 111.9(6) . .
C2B Si2 C4A 83.1(6) . .
C4B Si2 C4A 66.0(8) . .
C4B Si2 C4A 162.2(7) 14_755 .
C4A Si2 C4A 111.4(14) 14_755 .
C2A Si2 C3A 111.7(9) . .
C2B Si2 C3A 165.4(9) . .
C4B Si2 C3A 61.0(6) . .
C4B Si2 C3A 61.0(6) 14_755 .
C4A Si2 C3A 104.8(6) 14_755 .
C4A Si2 C3A 104.8(6) . .
C2A Si2 C3B 163.6(8) . .
C2B Si2 C3B 109.9(8) . .
C4B Si2 C3B 104.4(6) . .
C4B Si2 C3B 104.4(6) 14_755 .
C4A Si2 C3B 61.5(7) 14_755 .
C4A Si2 C3B 61.5(7) . .
C3A Si2 C3B 84.6(9) . .
C1 O1 U1 180.0 . .
O2 Li1 O2 27.2(12) 6_575 9_675
O2 Li1 O2 180.0(7) 6_575 14_655
O2 Li1 O2 152.8(12) 9_675 14_655
O2 Li1 O2 91.2(9) 6_575 5_655
O2 Li1 O2 84.9(10) 9_675 5_655
O2 Li1 O2 88.8(10) 14_655 5_655
O2 Li1 O2 84.9(10) 6_575 10
O2 Li1 O2 91.2(10) 9_675 10
O2 Li1 O2 95.1(10) 14_655 10
O2 Li1 O2 27.2(12) 5_655 10
O2 Li1 O2 95.1(10) 6_575 2_675
O2 Li1 O2 88.8(10) 9_675 2_675
O2 Li1 O2 84.9(10) 14_655 2_675
O2 Li1 O2 152.8(12) 5_655 2_675
O2 Li1 O2 180.0(11) 10 2_675
O2 Li1 O2 152.8(12) 6_575 .
O2 Li1 O2 180.000(3) 9_675 .
O2 Li1 O2 27.2(12) 14_655 .
O2 Li1 O2 95.1(10) 5_655 .
O2 Li1 O2 88.8(10) 10 .
O2 Li1 O2 91.2(9) 2_675 .
O2 Li1 O2 88.8(10) 6_575 13_575
O2 Li1 O2 95.1(10) 9_675 13_575
O2 Li1 O2 91.2(10) 14_655 13_575
O2 Li1 O2 180.000(2) 5_655 13_575
O2 Li1 O2 152.8(12) 10 13_575
O2 Li1 O2 27.2(12) 2_675 13_575
O2 Li1 O2 84.9(10) . 13_575
O2 Li1 O3 69.8(7) 6_575 13_575
O2 Li1 O3 96.8(7) 9_675 13_575
O2 Li1 O3 110.2(7) 14_655 13_575
O2 Li1 O3 110.2(7) 5_655 13_575
O2 Li1 O3 83.2(7) 10 13_575
O2 Li1 O3 96.8(7) 2_675 13_575
O2 Li1 O3 83.2(7) . 13_575
O2 Li1 O3 69.8(7) 13_575 13_575
O2 Li1 O3 110.2(7) 6_575 5_655
O2 Li1 O3 83.2(7) 9_675 5_655
O2 Li1 O3 69.8(7) 14_655 5_655
O2 Li1 O3 69.8(7) 5_655 5_655
O2 Li1 O3 96.8(7) 10 5_655
O2 Li1 O3 83.2(7) 2_675 5_655
O2 Li1 O3 96.8(7) . 5_655
O2 Li1 O3 110.2(7) 13_575 5_655
O3 Li1 O3 180.000(1) 13_575 5_655
O2 Li1 O3 96.8(7) 6_575 9_675
O2 Li1 O3 69.8(7) 9_675 9_675
O2 Li1 O3 83.2(7) 14_655 9_675
O2 Li1 O3 83.2(7) 5_655 9_675
O2 Li1 O3 110.2(7) 10 9_675
O2 Li1 O3 69.8(7) 2_675 9_675
O2 Li1 O3 110.2(7) . 9_675
O2 Li1 O3 96.8(7) 13_575 9_675
O3 Li1 O3 160.6(10) 13_575 9_675
O3 Li1 O3 19.4(10) 5_655 9_675
O2 Li1 O3 83.2(7) 6_575 .
O2 Li1 O3 110.2(7) 9_675 .
O2 Li1 O3 96.8(7) 14_655 .
O2 Li1 O3 96.8(7) 5_655 .
O2 Li1 O3 69.8(7) 10 .
O2 Li1 O3 110.2(7) 2_675 .
O2 Li1 O3 69.8(7) . .
O2 Li1 O3 83.2(7) 13_575 .
O3 Li1 O3 19.4(10) 13_575 .
O3 Li1 O3 160.6(10) 5_655 .
O3 Li1 O3 180.0 9_675 .
O1 C1 C6 107.2(8) . 10
O1 C1 C6 107.2(8) . 6_565
C6 C1 C6 109.7(19) 10 6_565
O1 C1 C6 107.2(8) . 13_565
C6 C1 C6 145.6(15) 10 13_565
C6 C1 C6 59(2) 6_565 13_565
O1 C1 C6 107.2(8) . .
C6 C1 C6 59(2) 10 .
C6 C1 C6 145.6(15) 6_565 .
C6 C1 C6 109.7(19) 13_565 .
O1 C1 C5 107.9(10) . .
C6 C1 C5 112.3(11) 10 .
C6 C1 C5 112.3(11) 6_565 .
C6 C1 C5 55.9(10) 13_565 .
C6 C1 C5 55.9(10) . .
O1 C1 C5 107.9(10) . 10
C6 C1 C5 55.9(10) 10 10
C6 C1 C5 55.9(10) 6_565 10
C6 C1 C5 112.3(11) 13_565 10
C6 C1 C5 112.3(11) . 10
C5 C1 C5 144(2) . 10
C2B C2A Si2 63.2(8) . .
C2B C2A U1 71.7(7) . .
Si2 C2A U1 134.9(8) . .
C2A C2B Si2 63.1(7) . .
C2A C2B U1 69.9(8) . .
Si2 C2B U1 133.0(8) . .
C4B C3A C4B 104.3(12) 14_755 .
C4B C3A Si2 57.1(6) 14_755 .
C4B C3A Si2 57.1(6) . .
C4A C3B C4A 103.5(12) . 14_755
C4A C3B Si2 56.7(7) . .
C4A C3B Si2 56.7(7) 14_755 .
Si2 C4B C3A 62.0(7) . .
Si2 C4B C4A 57.1(7) . .
C3A C4B C4A 99.5(11) . .
Si2 C4A C3B 61.7(8) . .
Si2 C4A C4B 56.9(7) . .
C3B C4A C4B 98.5(11) . .
C5 C6 C6 121.7(13) . 10
C5 C6 C1 64.7(11) . .
C6 C6 C1 60.4(10) 10 .
C6 C5 C6 117(3) . 13_565
C6 C5 C1 59.4(12) . .
C6 C5 C1 59.4(12) 13_565 .
C22 O10 C22 90.4(3) 12_656 .
C22 O10 C22 90.4(3) 12_656 2_665
C22 O10 C22 170(4) . 2_665
C22 O10 C22 170(4) 12_656 11_566
C22 O10 C22 90.4(3) . 11_566
C22 O10 C22 90.4(3) 2_665 11_566
O10 C22 C24 92(3) . 12_656
O10 C22 C24 92(3) . .
C24 C22 C24 169(4) 12_656 .
O10 C22 C22 44.79(17) . 12_656
C24 C22 C22 48(3) 12_656 12_656
C24 C22 C22 136(3) . 12_656
O10 C22 C22 44.79(16) . 11_566
C24 C22 C22 136(3) 12_656 11_566
C24 C22 C22 47(3) . 11_566
C22 C22 C22 89.2(7) 12_656 11_566
C22 C24 C22 85(5) 11_566 .
O2 C30 O2 48(2) . 14_655
O2 C30 C31 90(3) . 14_655
O2 C30 C31 45(2) 14_655 14_655
O3 C32 C31 112(4) . .
O3 C32 O3 21.8(13) . 13_575
C31 C32 O3 112(3) . 13_575
O3 C32 C32 62.6(15) . 13_575
C31 C32 C32 102(3) . 13_575
O3 C32 C32 40.7(9) 13_575 13_575
O3 C32 C32 41.3(14) . 10
C31 C32 C32 140(3) . 10
O3 C32 C32 56.5(9) 13_575 10
C32 C32 C32 90.000(1) 13_575 10
O3 O3 C32 117.4(15) 13_575 .
O3 O3 C32 117.4(15) 13_575 10
C32 O3 C32 97(3) . 10
O3 O3 C32 40.7(9) 13_575 6_575
C32 O3 C32 127(3) . 6_575
C32 O3 C32 77(2) 10 6_575
O3 O3 C32 40.7(9) 13_575 13_575
C32 O3 C32 77(2) . 13_575
C32 O3 C32 127(3) 10 13_575
C32 O3 C32 67.1(18) 6_575 13_575
O3 O3 Li1 80.3(5) 13_575 .
C32 O3 Li1 122.9(16) . .
C32 O3 Li1 122.9(16) 10 .
C32 O3 Li1 102.4(12) 6_575 .
C32 O3 Li1 102.4(12) 13_575 .
O2 C31 C32 100(4) . .
O2 O2 C30 66.2(12) 14_655 .
O2 O2 C31 149(3) 14_655 .
C30 O2 C31 97(3) . .
O2 O2 Li1 76.4(6) 14_655 .
C30 O2 Li1 142.0(18) . .
C31 O2 Li1 119(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
U1 O1 2.053(8) .
U1 O1 2.053(8) 9_765
U1 C2A 2.467(15) 10
U1 C2A 2.467(15) 2_765
U1 C2A 2.467(15) 9_765
U1 C2A 2.467(15) .
U1 C2B 2.494(16) 10
U1 C2B 2.494(16) 2_765
U1 C2B 2.494(16) .
U1 C2B 2.494(16) 9_765
Si2 C2A 1.809(15) .
Si2 C2B 1.810(15) .
Si2 C4B 1.840(16) .
Si2 C4B 1.840(16) 14_755
Si2 C4A 1.845(16) 14_755
Si2 C4A 1.845(16) .
Si2 C3A 1.935(17) .
Si2 C3B 1.94(2) .
O1 C1 1.436(13) .
Li1 O2 2.099(19) 6_575
Li1 O2 2.099(19) 9_675
Li1 O2 2.099(19) 14_655
Li1 O2 2.099(19) 5_655
Li1 O2 2.099(19) 10
Li1 O2 2.099(19) 2_675
Li1 O2 2.099(19) .
Li1 O2 2.099(19) 13_575
Li1 O3 2.137(16) 13_575
Li1 O3 2.137(16) 5_655
Li1 O3 2.137(16) 9_675
Li1 O3 2.137(16) .
C1 C6 1.488(16) 10
C1 C6 1.488(16) 6_565
C1 C6 1.488(16) 13_565
C1 C6 1.488(16) .
C1 C5 1.56(2) .
C1 C5 1.56(2) 10
C2A C2B 1.63(2) .
C3A C4B 1.92(2) 14_755
C3A C4B 1.92(2) .
C3B C4A 1.94(2) .
C3B C4A 1.94(2) 14_755
C4B C4A 2.01(2) .
C6 C5 1.43(3) .
C6 C6 1.47(5) 10
C5 C6 1.43(3) 13_565
O10 C22 1.39(5) 12_656
O10 C22 1.39(5) .
O10 C22 1.39(5) 2_665
O10 C22 1.39(5) 11_566
C22 C24 1.46(5) 12_656
C22 C24 1.46(5) .
C22 C22 1.97(6) 12_656
C22 C22 1.97(6) 11_566
C24 C22 1.46(5) 11_566
C30 O2 1.22(3) .
C30 O2 1.22(3) 14_655
C30 C31 1.99(6) 14_655
C32 O3 1.26(3) .
C32 C31 1.61(5) .
C32 O3 1.72(3) 13_575
C32 C32 1.88(5) 13_575
C32 C32 1.90(5) 10
O3 O3 0.72(4) 13_575
O3 C32 1.26(3) 10
O3 C32 1.72(3) 6_575
O3 C32 1.72(3) 13_575
C31 O2 1.43(7) .
O2 O2 0.99(4) 14_655
