#------------------------------------------------------------------------------
#$Date: 2016-03-22 23:58:59 +0200 (Tue, 22 Mar 2016) $
#$Revision: 179087 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/49/4304955.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_4304955
loop_
_publ_author_name
'Skye Fortier'
'Guang Wu'
'Trevor W. Hayton'
_publ_contact_author_email       hayton@chem.ucsb.edu
_publ_contact_author_name        'Trevor W. Hayton'
_publ_section_title
;
Synthesis and Characterization of Three Homoleptic Alkoxides of Uranium:
[Li(THF)]2[UIV(OtBu)6], [Li(Et2O)][UV(OtBu)6], and UVI(OtBu)6
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4752
_journal_page_last               4761
_journal_paper_doi               10.1021/ic800067k
_journal_volume                  47
_journal_year                    2008
_chemical_formula_sum            'C24 H54 O6 U'
_chemical_formula_weight         676.70
_chemical_name_systematic
; 
U(VI) hexakis(tert-butoxide) 
;
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/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                 93.80(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            6
_cell_length_a                   28.536(6)
_cell_length_b                   16.791(3)
_cell_length_c                   9.7246(19)
_cell_measurement_temperature    150(2)
_cell_volume                     4649.3(16)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.968
_diffrn_measured_fraction_theta_max 0.968
_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  0.1275
_diffrn_reflns_av_sigmaI/netI    0.1425
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            19563
_diffrn_reflns_theta_full        26.72
_diffrn_reflns_theta_max         27.71
_diffrn_reflns_theta_min         1.41
_exptl_absorpt_coefficient_mu    5.266
_exptl_absorpt_correction_T_max  0.327
_exptl_absorpt_correction_T_min  0.185
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Psi Scan'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.450
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2028
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.602
_refine_diff_density_min         -1.311
_refine_diff_density_rms         0.183
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.911
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     170
_refine_ls_number_reflns         4954
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      0.912
_refine_ls_R_factor_all          0.1176
_refine_ls_R_factor_gt           0.0537
_refine_ls_shift/su_max          0.021
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0585P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1206
_refine_ls_wR_factor_ref         0.1393
_reflns_number_gt                2699
_reflns_number_total             5097
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic800067k-file002_4.cif
_cod_data_source_block           c:\xtal\sf_2_b35\work\sf_2_b3m
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Empirical' changed to
'empirical' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        4649.4(16)
_cod_database_code               4304955
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -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
_atom_site_disorder_assembly
_atom_site_disorder_group
U1 U 0.5000 0.5000 0.5000 0.0370(2) Uani 1 4 d S . .
U2 U 0.832500(19) 0.5000 0.90552(5) 0.03859(19) Uani 1 2 d S . .
O3 O 0.7976(3) 0.5869(5) 0.7903(8) 0.075(3) Uani 1 1 d . . .
O4 O 0.7796(4) 0.5000 1.0424(14) 0.076(4) Uani 1 2 d S . .
O5 O 0.8673(3) 0.5861(6) 1.0231(10) 0.091(3) Uani 1 1 d . . .
O2 O 0.5417(3) 0.5843(5) 0.4223(9) 0.088(3) Uani 1 1 d . . .
O6 O 0.8872(4) 0.5000 0.7717(14) 0.087(4) Uani 1 2 d S . .
O1 O 0.5411(5) 0.5000 0.6815(14) 0.090(4) Uani 1 2 d S . .
C3 C 0.7781(4) 0.6421(7) 0.6990(14) 0.064(3) Uani 1 1 d . . .
C5 C 0.8831(5) 0.6433(7) 1.1082(13) 0.083(4) Uani 1 1 d D . .
C6 C 0.9256(7) 0.5000 0.701(2) 0.085(6) Uani 1 2 d SD . .
C1 C 0.5710(8) 0.5000 0.790(3) 0.098(7) Uani 1 2 d S . .
C4 C 0.7406(9) 0.5000 1.116(2) 0.098(7) Uani 1 2 d S . .
C2 C 0.5673(6) 0.6472(9) 0.3726(16) 0.095(5) Uani 1 1 d . . .
C14 C 0.8064(8) 0.6440(13) 0.577(3) 0.158(8) Uiso 1 1 d . . .
C15 C 0.7124(8) 0.5732(15) 1.074(3) 0.173(9) Uiso 1 1 d . . .
C12 C 0.7299(9) 0.6235(14) 0.655(3) 0.169(9) Uiso 1 1 d . . .
C13 C 0.7829(9) 0.7200(16) 0.757(3) 0.183(10) Uiso 1 1 d . . .
C11 C 0.6080(11) 0.6188(18) 0.318(3) 0.212(12) Uiso 1 1 d . . .
C10 C 0.5821(10) 0.7000(19) 0.485(3) 0.214(12) Uiso 1 1 d . . .
C9 C 0.5386(10) 0.6888(19) 0.263(4) 0.221(12) Uiso 1 1 d . . .
C7 C 0.5692(11) 0.570(2) 0.869(4) 0.244(14) Uiso 1 1 d . . .
C17 C 0.9249(9) 0.6932(19) 1.080(3) 0.155(7) Uiso 0.50 1 d PD . .
C16 C 0.7501(16) 0.5000 1.259(5) 0.24(2) Uiso 1 2 d S . .
C19 C 0.8989(13) 0.6120(18) 1.248(2) 0.155(7) Uiso 0.50 1 d PD . .
C8 C 0.6156(17) 0.5000 0.723(5) 0.24(2) Uiso 1 2 d S . .
C24 C 0.9445(12) 0.5822(11) 0.677(4) 0.117(12) Uiso 0.50 1 d PD . .
C23 C 0.9169(17) 0.543(3) 0.567(3) 0.19(2) Uiso 0.50 1 d PD . .
C25 C 0.9622(12) 0.544(2) 0.791(4) 0.171(19) Uiso 0.50 1 d PD . .
C21 C 0.8504(11) 0.7073(18) 1.149(4) 0.155(7) Uiso 0.50 1 d PD . .
C22 C 0.8835(13) 0.7292(11) 1.070(4) 0.155(7) Uiso 0.50 1 d PD . .
C20 C 0.8581(12) 0.649(2) 1.238(3) 0.155(7) Uiso 0.50 1 d PD . .
C18 C 0.9322(7) 0.6351(19) 1.169(3) 0.155(7) 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'
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
_geom_angle_publ_flag
O2 U1 O2 91.4(6) 5_666 6_565 ?
O2 U1 O2 88.6(6) 5_666 2_656 ?
O2 U1 O2 180.0(4) 6_565 2_656 ?
O2 U1 O2 180.0(4) 5_666 . ?
O2 U1 O2 88.6(6) 6_565 . ?
O2 U1 O2 91.4(6) 2_656 . ?
O2 U1 O1 89.7(4) 5_666 . ?
O2 U1 O1 90.3(4) 6_565 . ?
O2 U1 O1 89.7(4) 2_656 . ?
O2 U1 O1 90.3(4) . . ?
O2 U1 O1 90.3(4) 5_666 5_666 ?
O2 U1 O1 89.7(4) 6_565 5_666 ?
O2 U1 O1 90.3(4) 2_656 5_666 ?
O2 U1 O1 89.7(4) . 5_666 ?
O1 U1 O1 180.000(2) . 5_666 ?
O3 U2 O3 90.4(5) 6_565 . ?
O3 U2 O5 179.3(4) 6_565 . ?
O3 U2 O5 90.1(4) . . ?
O3 U2 O5 90.1(4) 6_565 6_565 ?
O3 U2 O5 179.3(4) . 6_565 ?
O5 U2 O5 89.3(6) . 6_565 ?
O3 U2 O4 90.2(3) 6_565 . ?
O3 U2 O4 90.2(3) . . ?
O5 U2 O4 89.3(4) . . ?
O5 U2 O4 89.3(4) 6_565 . ?
O3 U2 O6 90.9(3) 6_565 . ?
O3 U2 O6 90.9(3) . . ?
O5 U2 O6 89.6(4) . . ?
O5 U2 O6 89.6(4) 6_565 . ?
O4 U2 O6 178.5(5) . . ?
C3 O3 U2 172.2(8) . . ?
C4 O4 U2 171.7(13) . . ?
C5 O5 U2 170.6(9) . . ?
C2 O2 U1 174.8(11) . . ?
C6 O6 U2 172.7(13) . . ?
C1 O1 U1 174.2(15) . . ?
O3 C3 C12 112.4(14) . . ?
O3 C3 C13 109.6(15) . . ?
C12 C3 C13 112.4(17) . . ?
O3 C3 C14 108.1(13) . . ?
C12 C3 C14 109.3(17) . . ?
C13 C3 C14 104.7(16) . . ?
O5 C5 C21 119.6(19) . . ?
O5 C5 C22 123.4(19) . . ?
C21 C5 C22 52.2(5) . . ?
O5 C5 C18 116.9(16) . . ?
C21 C5 C18 123.2(16) . . ?
C22 C5 C18 99.5(10) . . ?
O5 C5 C20 114.3(18) . . ?
C21 C5 C20 52.4(5) . . ?
C22 C5 C20 99.5(14) . . ?
C18 C5 C20 99.0(10) . . ?
O5 C5 C19 112.4(17) . . ?
C21 C5 C19 99.6(13) . . ?
C22 C5 C19 124.1(18) . . ?
C18 C5 C19 52.3(5) . . ?
C20 C5 C19 52.1(5) . . ?
O5 C5 C17 122.1(17) . . ?
C21 C5 C17 99.5(13) . . ?
C22 C5 C17 52.6(5) . . ?
C18 C5 C17 52.1(5) . . ?
C20 C5 C17 123.4(18) . . ?
C19 C5 C17 99.6(8) . . ?
O6 C6 C25 105(2) . . ?
O6 C6 C25 105(2) . 6_565 ?
C25 C6 C25 58(3) . 6_565 ?
O6 C6 C23 111(2) . . ?
C25 C6 C23 109(3) . . ?
C25 C6 C23 144(3) 6_565 . ?
O6 C6 C23 111(2) . 6_565 ?
C25 C6 C23 144(3) . 6_565 ?
C25 C6 C23 109(3) 6_565 6_565 ?
C23 C6 C23 58(4) . 6_565 ?
O6 C6 C24 113.3(16) . . ?
C25 C6 C24 53(2) . . ?
C25 C6 C24 107(3) 6_565 . ?
C23 C6 C24 57(2) . . ?
C23 C6 C24 110(3) 6_565 . ?
O6 C6 C24 113.3(16) . 6_565 ?
C25 C6 C24 107(3) . 6_565 ?
C25 C6 C24 53(2) 6_565 6_565 ?
C23 C6 C24 110(3) . 6_565 ?
C23 C6 C24 57(2) 6_565 6_565 ?
C24 C6 C24 133(3) . 6_565 ?
O1 C1 C7 113.1(19) . 6_565 ?
O1 C1 C7 113.1(19) . . ?
C7 C1 C7 113(4) 6_565 . ?
O1 C1 C8 100(3) . . ?
C7 C1 C8 108(2) 6_565 . ?
C7 C1 C8 108(2) . . ?
O4 C4 C16 114(3) . . ?
O4 C4 C15 107.4(15) . 6_565 ?
C16 C4 C15 109.3(18) . 6_565 ?
O4 C4 C15 107.4(15) . . ?
C16 C4 C15 109.3(18) . . ?
C15 C4 C15 109(2) 6_565 . ?
C11 C2 O2 110.1(19) . . ?
C11 C2 C10 107(2) . . ?
O2 C2 C10 109.7(17) . . ?
C11 C2 C9 109(2) . . ?
O2 C2 C9 109.3(17) . . ?
C10 C2 C9 112(2) . . ?
C18 C17 C5 63.6(6) . . ?
C18 C17 C22 119.3(14) . . ?
C5 C17 C22 63.4(6) . . ?
C20 C19 C18 119.1(14) . . ?
C20 C19 C5 63.7(6) . . ?
C18 C19 C5 63.5(6) . . ?
C25 C24 C23 123.3(17) . . ?
C25 C24 C6 63.3(11) . . ?
C23 C24 C6 61.3(12) . . ?
C24 C23 C6 61.4(12) . . ?
C24 C23 C23 116.8(17) . 6_565 ?
C6 C23 C23 61.0(19) . 6_565 ?
C24 C25 C6 63.4(12) . . ?
C24 C25 C25 118.6(18) . 6_565 ?
C6 C25 C25 60.8(17) . 6_565 ?
C22 C21 C20 120.0(19) . . ?
C22 C21 C5 63.8(6) . . ?
C20 C21 C5 63.9(6) . . ?
C21 C22 C5 64.0(6) . . ?
C21 C22 C17 120.1(19) . . ?
C5 C22 C17 64.0(6) . . ?
C19 C20 C21 120.4(18) . . ?
C19 C20 C5 64.2(6) . . ?
C21 C20 C5 63.8(6) . . ?
C17 C18 C19 121.1(11) . . ?
C17 C18 C5 64.2(6) . . ?
C19 C18 C5 64.2(6) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
U1 O2 2.027(8) 5_666 ?
U1 O2 2.027(8) 6_565 ?
U1 O2 2.027(8) 2_656 ?
U1 O2 2.027(8) . ?
U1 O1 2.052(13) . ?
U1 O1 2.052(13) 5_666 ?
U2 O3 2.056(8) 6_565 ?
U2 O3 2.056(8) . ?
U2 O5 2.057(9) . ?
U2 O5 2.057(8) 6_565 ?
U2 O4 2.077(13) . ?
U2 O6 2.098(14) . ?
O3 C3 1.376(13) . ?
O4 C4 1.36(2) . ?
O5 C5 1.327(12) . ?
O2 C2 1.390(15) . ?
O6 C6 1.33(2) . ?
O1 C1 1.31(2) . ?
C3 C12 1.44(2) . ?
C3 C13 1.43(3) . ?
C3 C14 1.48(3) . ?
C5 C21 1.494(10) . ?
C5 C22 1.491(10) . ?
C5 C18 1.491(10) . ?
C5 C20 1.495(10) . ?
C5 C19 1.501(10) . ?
C5 C17 1.499(10) . ?
C6 C25 1.505(10) . ?
C6 C25 1.505(10) 6_565 ?
C6 C23 1.504(10) . ?
C6 C23 1.504(10) 6_565 ?
C6 C24 1.506(10) . ?
C6 C24 1.506(10) 6_565 ?
C1 C7 1.41(3) 6_565 ?
C1 C7 1.41(3) . ?
C1 C8 1.47(5) . ?
C4 C16 1.40(5) . ?
C4 C15 1.51(3) 6_565 ?
C4 C15 1.51(3) . ?
C2 C11 1.39(3) . ?
C2 C10 1.45(3) . ?
C2 C9 1.48(3) . ?
C17 C18 1.314(10) . ?
C17 C22 1.324(10) . ?
C19 C20 1.317(10) . ?
C19 C18 1.319(10) . ?
C24 C25 1.35(5) . ?
C24 C23 1.44(5) . ?
C23 C23 1.46(9) 6_565 ?
C25 C25 1.47(8) 6_565 ?
C21 C22 1.312(10) . ?
C21 C20 1.319(10) . ?
