Activation and reduction of diethyl ether by low valent uranium: formation of the trimetallic, mixed valence uranium oxo species [U(CpRR')(μ-I)2]3(μ3-O) (CpRR' = C5Me5, C5Me4H, C5H4SiMe3)
Larch, Christopher P.; Cloke, F. Geoffrey N.; Hitchcock, Peter B.; Chemical Communications (Cambridge, United Kingdom)  (2008) 82–84; doi:10.1039/b714211k

data_7102774
_publ_section_title
;
 Activation and reduction of diethyl ether by low valent uranium:
 formation of the trimetallic, mixed valence uranium oxo species
 [U(CpRR')(\m-I)2]3(\m3-O) (CpRR' = C5Me5, C5Me4H, C5H4SiMe3)
;
_journal_coden_ASTM              CHCOFS
_journal_issue                   1
_journal_name_full
;
 Chemical Communications (Cambridge, United Kingdom)
;
_journal_page_first              82
_journal_page_last               84
_journal_paper_doi               10.1039/b714211k
_journal_year                    2008
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C30 H45 I6 O U3'
_chemical_formula_sum            'C30 H45 I6 O U3'
_chemical_formula_weight         1897.15
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.2
_audit_creation_date             2007-07-31T13:45:24-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 109.891(1)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   24.5979(5)
_cell_length_b                   21.5504(4)
_cell_length_c                   16.6282(3)
_cell_measurement_reflns_used    167899
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      24.713
_cell_measurement_theta_min      3.705
_cell_measurement_wavelength     0.71073
_cell_volume                     8288.7(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.95
_diffrn_measured_fraction_theta_max 0.95
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0924
_diffrn_reflns_av_unetI/netI     0.0617
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            55482
_diffrn_reflns_theta_full        24.67
_diffrn_reflns_theta_max         24.67
_diffrn_reflns_theta_min         3.72
_exptl_absorpt_coefficient_mu    16.185
_exptl_absorpt_correction_T_max  0.3167
_exptl_absorpt_correction_T_min  0.2226
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    3.041
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             6616
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.257
_refine_diff_density_min         -2.546
_refine_diff_density_rms         0.355
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     442
_refine_ls_number_reflns         13374
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0583
_refine_ls_R_factor_gt           0.0482
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0499P)^2^+114.3734P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1128
_refine_ls_wR_factor_ref         0.1189
_reflns_number_gt                11825
_reflns_number_total             13374
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b714211k.txt
_cod_data_source_block           jan703
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7102774