Synthesis and Characterization of Three Homoleptic Alkoxides of Uranium: [Li(THF)]2[UIV(OtBu)6], [Li(Et2O)][UV(OtBu)6], and UVI(OtBu)6
Skye Fortier; Guang Wu; Trevor W. Hayton; Inorganic Chemistry 47 (2008) 4752–4761; doi:10.1021/ic800067k

data_4304955
_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
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_diffrn_reflns_limit_h_min       -31
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_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
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_refine_ls_number_reflns         4954
_refine_ls_number_restraints     18
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_refine_ls_R_factor_all          0.1176
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_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/[\s^2^(Fo^2^)+(0.0585P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/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