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_4304954
_publ_contact_author_email       hayton@chem.ucsb.edu
_publ_contact_author_name        'Trevor W. Hayton'
_publ_section_title
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Synthesis and Characterization of Three Homoleptic Alkoxides of Uranium:
[Li(THF)]2[UIV(OtBu)6], [Li(Et2O)][UV(OtBu)6], and UVI(OtBu)6
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_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            'C28 H64 Li O7 U'
_chemical_formula_weight         757.76
_chemical_name_systematic
; 
Lithium diethyl ether Uranium(V) hexakis(tert-butoxide) 
;
_space_group_IT_number           44
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'I 2 -2'
_symmetry_space_group_name_H-M   'I m m 2'
_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                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.18(2)
_cell_length_b                   12.41(3)
_cell_length_c                   13.19(3)
_cell_measurement_temperature    150(2)
_cell_volume                     1830(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 0.969
_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  0.1118
_diffrn_reflns_av_sigmaI/netI    0.0653
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            7142
_diffrn_reflns_theta_full        26.73
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.25
_exptl_absorpt_coefficient_mu    4.471
_exptl_absorpt_correction_T_max  0.393
_exptl_absorpt_correction_T_min  0.153
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Psi Scan'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.376
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       hexagon
_exptl_crystal_F_000             766
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.319
_refine_diff_density_min         -2.075
_refine_diff_density_rms         0.135
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.76(3)
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     127
_refine_ls_number_reflns         1999
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_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.0352
_refine_ls_R_factor_gt           0.0352
_refine_ls_shift/su_max          0.100
_refine_ls_shift/su_mean         0.016
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0311P)^2^+10.5827P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0873
_refine_ls_wR_factor_ref         0.0873
_reflns_number_gt                2024
_reflns_number_total             2024
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic800067k-file002_3.cif
_cod_data_source_block           sf_2_97
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
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 
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_cod_original_cell_volume        1829(7)
_cod_database_code               4304954