#------------------------------------------------------------------------------
#$Date: 2016-03-21 16:59:44 +0100 (lun 21 de mar de 2016) $
#$Revision: 178798 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/52/4105200.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_4105200
loop_
_publ_author_name
'Skye Fortier'
'Brent C. Melot'
'Guang Wu'
'Trevor W. Hayton'
_publ_contact_author_email       hayton@chem.ucsb.edu
_publ_contact_author_name        'Trevor W. Hayton'
_publ_section_title
;
 Homoleptic Uranium(IV) Alkyl Complexes: Synthesis and Characterization
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              15512
_journal_page_last               15521
_journal_paper_doi               10.1021/ja906516e
_journal_volume                  131
_journal_year                    2009
_chemical_formula_sum            'C41 H37 Li O4 U'
_chemical_formula_weight         838.68
_chemical_name_systematic
; 
 Lithium tetrakis(tetrahydrofuran) pentakis(neopentyl) uranium(IV) 
;
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 1'
_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                 103.390(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.4775(13)
_cell_length_b                   16.944(2)
_cell_length_c                   13.7753(17)
_cell_measurement_temperature    150(2)
_cell_volume                     2379.1(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.969
_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  0.1331
_diffrn_reflns_av_sigmaI/netI    0.0796
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            19784
_diffrn_reflns_theta_full        26.73
_diffrn_reflns_theta_max         26.73
_diffrn_reflns_theta_min         1.52
_exptl_absorpt_coefficient_mu    3.441
_exptl_absorpt_correction_T_max  0.410
_exptl_absorpt_correction_T_min  0.195
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Psi Scan'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.171
_exptl_crystal_description       block
_exptl_crystal_F_000             820
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.25
_refine_diff_density_max         2.725
_refine_diff_density_min         -2.639
_refine_diff_density_rms         0.265
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     289
_refine_ls_number_reflns         5067
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.106
_refine_ls_R_factor_all          0.0663
_refine_ls_R_factor_gt           0.0534
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0988P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1377
_refine_ls_wR_factor_ref         0.1580
_reflns_number_gt                4313
_reflns_number_total             5067
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja906516e_si_001_3.cif
_cod_data_source_block           Complex_3
_cod_original_cell_volume        2379.0(5)
_cod_database_code               4105200
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x, -y-1/2, z'
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 0.73212(3) 0.7500 0.72304(2) 0.03336(15) Uani 1 2 d S
C3 C 0.9441(12) 0.7753(8) 0.8469(10) 0.046(4) Uani 0.50 1 d P
C4 C 0.5657(9) 0.9003(6) 0.8443(6) 0.062(2) Uani 1 1 d .
C8 C 0.7467(13) 0.9025(6) 0.5283(8) 0.082(3) Uani 1 1 d .
C12 C 1.0849(10) 0.7500 0.8516(9) 0.051(3) Uani 1 2 d S
C13 C 1.1336(15) 0.7500 0.7650(12) 0.139(10) Uani 1 2 d S
C14 C 1.1820(15) 0.7734(10) 0.9469(13) 0.057(5) Uani 0.50 1 d P
C15 C 1.0816(19) 0.8464(9) 0.8608(19) 0.084(7) Uani 0.50 1 d P
C20 C 0.3658(15) 0.8224(13) 0.1995(14) 0.140(4) Uani 1 1 d .
C21 C 0.4933(14) 0.7880(10) 0.1877(13) 0.140(4) Uani 1 1 d .
C22 C 0.153(4) 0.8106(13) 0.455(2) 0.124(14) Uani 0.50 1 d P
C23 C 0.243(3) 0.8268(15) 0.530(2) 0.099(8) Uani 0.50 1 d P
C24 C 0.310(2) 0.7500 0.5423(15) 0.101(6) Uani 1 2 d S
C25 C 0.281(4) 0.801(2) 0.448(3) 0.146(15) Uani 0.50 1 d P
C1B C 0.5508(12) 0.8295(7) 0.7615(9) 0.043(3) Uani 0.562(9) 1 d P
C2A C 0.7845(14) 0.8572(8) 0.6124(11) 0.049(3) Uani 0.562(9) 1 d P
C5A C 0.481(4) 0.935(2) 0.7445(18) 0.176(19) Uani 0.562(9) 1 d P
C6A C 0.629(3) 0.9878(13) 0.904(3) 0.127(11) Uani 0.562(9) 1 d P
C7A C 0.497(3) 0.8688(15) 0.907(2) 0.110(10) Uani 0.562(9) 1 d P
C10A C 0.644(2) 0.9779(13) 0.563(2) 0.111(10) Uani 0.562(9) 1 d P
C11A C 0.826(2) 0.9572(12) 0.4844(17) 0.085(6) Uani 0.562(9) 1 d P
C1A C 0.6800(15) 0.8593(8) 0.8261(11) 0.034(3) Uani 0.438(9) 1 d P
C2B C 0.6759(15) 0.8352(9) 0.5733(11) 0.038(3) Uani 0.438(9) 1 d P
C5B C 0.675(2) 0.9494(11) 0.8469(16) 0.058(5) Uani 0.438(9) 1 d P
C6B C 0.598(3) 0.8474(12) 0.9482(14) 0.057(5) Uani 0.438(9) 1 d P
C7B C 0.4382(17) 0.9374(11) 0.8391(16) 0.058(5) Uani 0.438(9) 1 d P
C9B C 0.699(2) 0.9291(13) 0.4325(15) 0.065(6) Uani 0.438(9) 1 d P
C10B C 0.892(3) 0.8498(14) 0.523(2) 0.080(8) Uani 0.438(9) 1 d P
C11B C 0.793(4) 0.9649(15) 0.610(2) 0.115(14) Uani 0.438(9) 1 d P
Li1 Li 0.126(3) 0.7500 0.248(2) 0.093(8) Uani 1 2 d S
O1 O 0.1638(12) 0.7500 0.3906(8) 0.083(3) Uani 1 2 d S
O3 O 0.2938(15) 0.7500 0.2117(14) 0.140(4) Uani 1 2 d S
C9A C 0.623(4) 0.8669(13) 0.4408(18) 0.152(15) Uani 0.562(9) 1 d P
C31 C -0.073(2) 0.9675(12) 0.1165(13) 0.217(6) Uani 1 1 d D
C30 C 0.012(2) 0.8962(13) 0.1150(14) 0.217(6) Uani 1 1 d D
C32 C -0.1386(18) 0.9446(15) 0.1969(13) 0.217(6) Uani 1 1 d D
C33 C -0.034(2) 0.8955(13) 0.2617(11) 0.217(6) Uani 1 1 d D
O2 O 0.0232(16) 0.8477(10) 0.1986(9) 0.217(6) Uani 1 1 d D
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'
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
C1A U1 C1A 97.1(6) . 4_575
C1A U1 C2B 151.0(5) . 4_575
C1A U1 C2B 90.0(5) 4_575 4_575
C1A U1 C2B 90.0(5) . .
C1A U1 C2B 151.0(5) 4_575 .
C2B U1 C2B 71.4(7) 4_575 .
C1A U1 C1B 90.1(5) . 4_575
C1A U1 C1B 35.8(5) 4_575 4_575
C2B U1 C1B 79.4(5) 4_575 4_575
C2B U1 C1B 116.6(5) . 4_575
C1A U1 C1B 35.8(5) . .
C1A U1 C1B 90.1(5) 4_575 .
C2B U1 C1B 116.6(5) 4_575 .
C2B U1 C1B 79.4(4) . .
C1B U1 C1B 65.7(6) 4_575 .
C1A U1 C3 76.1(5) . .
C1A U1 C3 90.9(5) 4_575 .
C2B U1 C3 132.1(5) 4_575 .
C2B U1 C3 118.1(5) . .
C1B U1 C3 123.3(5) 4_575 .
C1B U1 C3 111.3(4) . .
C1A U1 C3 90.9(5) . 4_575
C1A U1 C3 76.1(5) 4_575 4_575
C2B U1 C3 118.1(5) 4_575 4_575
C2B U1 C3 132.1(5) . 4_575
C1B U1 C3 111.3(4) 4_575 4_575
C1B U1 C3 123.3(5) . 4_575
C3 U1 C3 19.7(6) . 4_575
C1A U1 C2A 177.6(4) . 4_575
C1A U1 C2A 85.1(5) 4_575 4_575
C2B U1 C2A 27.8(5) 4_575 4_575
C2B U1 C2A 87.7(5) . 4_575
C1B U1 C2A 91.3(4) 4_575 4_575
C1B U1 C2A 143.8(4) . 4_575
C3 U1 C2A 104.7(4) . 4_575
C3 U1 C2A 90.3(5) 4_575 4_575
C1A U1 C2A 85.1(5) . .
C1A U1 C2A 177.6(4) 4_575 .
C2B U1 C2A 87.7(5) 4_575 .
C2B U1 C2A 27.8(5) . .
C1B U1 C2A 143.8(4) 4_575 .
C1B U1 C2A 91.3(4) . .
C3 U1 C2A 90.3(5) . .
C3 U1 C2A 104.7(4) 4_575 .
C2A U1 C2A 92.6(7) 4_575 .
C3 C3 C12 73.6(5) 4_575 .
C3 C3 U1 80.1(3) 4_575 .
C12 C3 U1 132.7(8) . .
C7A C4 C5B 139.9(16) . .
C7A C4 C1A 120.2(16) . .
C5B C4 C1A 65.7(10) . .
C7A C4 C7B 65.5(16) . .
C5B C4 C7B 118.4(13) . .
C1A C4 C7B 167.1(12) . .
C7A C4 C5A 115(2) . .
C5B C4 C5A 95(2) . .
C1A C4 C5A 110.6(12) . .
C7B C4 C5A 57.9(14) . .
C7A C4 C1B 100.2(12) . .
C5B C4 C1B 113.3(10) . .
C1A C4 C1B 58.7(8) . .
C7B C4 C1B 110.0(10) . .
C5A C4 C1B 74.0(12) . .
C7A C4 C6B 42.9(15) . .
C5B C4 C6B 107.3(14) . .
C1A C4 C6B 83.2(11) . .
C7B C4 C6B 105.9(14) . .
C5A C4 C6B 157(2) . .
C1B C4 C6B 99.9(10) . .
C7A C4 C6A 103.7(14) . .
C5B C4 C6A 43.0(11) . .
C1A C4 C6A 104.2(12) . .
C7B C4 C6A 84.6(13) . .
C5A C4 C6A 99.6(19) . .
C1B C4 C6A 155.6(12) . .
C6B C4 C6A 94.4(15) . .
C2A C8 C9B 164.9(15) . .
C2A C8 C11A 128.6(15) . .
C9B C8 C11A 60.8(14) . .
C2A C8 C11B 77.6(14) . .
C9B C8 C11B 117.5(17) . .
C11A C8 C11B 75.7(14) . .
C2A C8 C2B 47.7(9) . .
C9B C8 C2B 121.2(14) . .
C11A C8 C2B 172.2(14) . .
C11B C8 C2B 108.0(12) . .
C2A C8 C9A 115.7(12) . .
C9B C8 C9A 51.2(14) . .
C11A C8 C9A 110.5(16) . .
C11B C8 C9A 147(2) . .
C2B C8 C9A 70.3(12) . .
C2A C8 C10B 70.8(11) . .
C9B C8 C10B 104.6(14) . .
C11A C8 C10B 74.2(12) . .
C11B C8 C10B 104(2) . .
C2B C8 C10B 98.0(11) . .
C9A C8 C10B 108.6(18) . .
C2A C8 C10A 104.3(11) . .
C9B C8 C10A 85.0(15) . .
C11A C8 C10A 95.2(12) . .
C11B C8 C10A 55.2(19) . .
C2B C8 C10A 92.5(10) . .
C9A C8 C10A 92.0(18) . .
C10B C8 C10A 159.0(16) . .
C13 C12 C14 115.7(11) . .
C13 C12 C14 115.7(11) . 4_575
C14 C12 C14 30.4(13) . 4_575
C13 C12 C3 120.3(11) . 4_575
C14 C12 C3 124.0(12) . 4_575
C14 C12 C3 114.3(11) 4_575 4_575
C13 C12 C3 120.3(11) . .
C14 C12 C3 114.3(11) . .
C14 C12 C3 124.0(12) 4_575 .
C3 C12 C3 32.7(10) 4_575 .
C13 C12 C15 94.8(10) . 4_575
C14 C12 C15 102.5(11) . 4_575
C14 C12 C15 72.2(10) 4_575 4_575
C3 C12 C15 71.6(9) 4_575 4_575
C3 C12 C15 104.3(10) . 4_575
C13 C12 C15 94.8(10) . .
C14 C12 C15 72.2(10) . .
C14 C12 C15 102.5(11) 4_575 .
C3 C12 C15 104.3(10) 4_575 .
C3 C12 C15 71.6(9) . .
C15 C12 C15 170(2) 4_575 .
C14 C14 C12 74.8(7) 4_575 .
O3 C20 C21 100.5(16) . .
C21 C21 C20 112.8(10) 4_575 .
C23 C22 O1 122(3) . .
C22 C23 C24 98(2) . .
C23 C24 C23 124(3) 4_575 .
C23 C24 C25 54(2) 4_575 4_575
C23 C24 C25 114(2) . 4_575
C23 C24 C25 114(2) 4_575 .
C23 C24 C25 54(2) . .
C25 C24 C25 68(3) 4_575 .
C24 C25 O1 96(2) . .
C24 C25 C25 56.0(16) . 4_575
O1 C25 C25 56.6(15) . 4_575
C1A C1B C4 54.7(7) . .
C1A C1B U1 71.6(7) . .
C4 C1B U1 126.3(7) . .
C2B C2A C8 74.7(11) . .
C2B C2A U1 74.3(9) . .
C8 C2A U1 149.0(10) . .
C7B C5A C4 57.3(12) . .
C5B C6A C4 53.3(13) . .
C6B C7A C4 82.5(16) . .
C6B C7A C7B 138(2) . .
C4 C7A C7B 60.4(15) . .
C11B C10A C8 53.8(11) . .
C9B C11A C8 56.5(12) . .
C4 C1A C1B 66.6(9) . .
C4 C1A C5B 55.7(10) . .
C1B C1A C5B 111.7(13) . .
C4 C1A U1 139.2(10) . .
C1B C1A U1 72.6(7) . .
C5B C1A U1 149.6(11) . .
C2A C2B C8 57.6(10) . .
C2A C2B U1 77.8(9) . .
C8 C2B U1 135.5(10) . .
C6A C5B C4 83.7(17) . .
C6A C5B C1A 133(2) . .
C4 C5B C1A 58.5(9) . .
C7A C6B C4 54.6(16) . .
C4 C7B C5A 64.8(12) . .
C4 C7B C7A 54.1(10) . .
C5A C7B C7A 111.6(14) . .
C9A C9B C8 75.6(15) . .
C9A C9B C11A 136(2) . .
C8 C9B C11A 62.7(13) . .
C8 C11B C10A 71.0(18) . .
O1 Li1 O3 106.4(17) . .
O1 Li1 O2 108.5(11) . 4_575
O3 Li1 O2 111.1(11) . 4_575
O1 Li1 O2 108.5(11) . .
O3 Li1 O2 111.1(11) . .
O2 Li1 O2 111.1(19) 4_575 .
C22 O1 C22 97(2) . 4_575
C22 O1 C25 56(2) . .
C22 O1 C25 105(2) 4_575 .
C22 O1 C25 105(2) . 4_575
C22 O1 C25 56(2) 4_575 4_575
C25 O1 C25 67(3) . 4_575
C22 O1 Li1 129.1(14) . .
C22 O1 Li1 129.1(14) 4_575 .
C25 O1 Li1 118.0(17) . .
C25 O1 Li1 118.0(17) 4_575 .
C20 O3 C20 113.1(19) . 4_575
C20 O3 Li1 123.4(10) . .
C20 O3 Li1 123.4(10) 4_575 .
C9B C9A C8 53.2(14) . .
C32 C31 C30 100.3(8) . .
O2 C30 C31 113.4(10) . .
C31 C32 C33 100.8(8) . .
O2 C33 C32 107.9(13) . .
C30 O2 C33 101.7(12) . .
C30 O2 Li1 134.5(13) . .
C33 O2 Li1 122.1(12) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
U1 C1A 2.470(14) .
U1 C1A 2.470(14) 4_575
U1 C2B 2.474(15) 4_575
U1 C2B 2.474(15) .
U1 C1B 2.485(13) 4_575
U1 C1B 2.485(13) .
U1 C3 2.505(12) .
U1 C3 2.505(12) 4_575
U1 C2A 2.512(13) 4_575
U1 C2A 2.512(13) .
C3 C3 0.86(3) 4_575
C3 C12 1.523(16) .
C4 C7A 1.36(3) .
C4 C5B 1.41(2) .
C4 C1A 1.457(16) .
C4 C7B 1.462(18) .
C4 C5A 1.57(2) .
C4 C1B 1.638(14) .
C4 C6B 1.66(2) .
C4 C6A 1.75(2) .
C8 C2A 1.370(17) .
C8 C9B 1.37(2) .
C8 C11A 1.46(2) .
C8 C11B 1.54(3) .
C8 C2B 1.565(17) .
C8 C9A 1.66(3) .
C8 C10B 1.78(3) .
C8 C10A 1.81(2) .
C12 C13 1.403(19) .
C12 C14 1.516(19) .
C12 C14 1.516(19) 4_575
C12 C3 1.523(16) 4_575
C12 C15 1.640(17) 4_575
C12 C15 1.640(17) .
C14 C14 0.79(3) 4_575
C20 O3 1.470(18) .
C20 C21 1.50(2) .
C21 C21 1.29(3) 4_575
C22 C23 1.27(5) .
C22 O1 1.37(3) .
C23 C24 1.47(3) .
C24 C23 1.47(3) 4_575
C24 C25 1.53(4) 4_575
C24 C25 1.53(4) .
C25 O1 1.56(4) .
C25 C25 1.71(7) 4_575
C1B C1A 1.52(2) .
C2A C2B 1.20(2) .
C5A C7B 1.47(3) .
C6A C5B 1.20(3) .
C7A C6B 1.14(3) .
C7A C7B 1.53(4) .
C10A C11B 1.57(5) .
C11A C9B 1.44(3) .
C1A C5B 1.56(2) .
C9B C9A 1.34(4) .
Li1 O1 1.91(3) .
Li1 O3 1.94(3) .
Li1 O2 2.01(2) 4_575
Li1 O2 2.01(2) .
O1 C22 1.37(3) 4_575
O1 C25 1.56(4) 4_575
O3 C20 1.470(18) 4_575
C31 C32 1.486(9) .
C31 C30 1.505(9) .
C30 O2 1.398(9) .
C32 C33 1.495(9) .
C33 O2 1.419(9) .
